CN1239574C - Macromolecule polymer and method for preparing the same - Google Patents
Macromolecule polymer and method for preparing the same Download PDFInfo
- Publication number
- CN1239574C CN1239574C CN 03116731 CN03116731A CN1239574C CN 1239574 C CN1239574 C CN 1239574C CN 03116731 CN03116731 CN 03116731 CN 03116731 A CN03116731 A CN 03116731A CN 1239574 C CN1239574 C CN 1239574C
- Authority
- CN
- China
- Prior art keywords
- hour
- temperature
- maintained
- polymer
- kept
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The present invention discloses a high molecular polymer which is characterized in that dicyandiamine and ammonia chloride are adopted and synthesized to obtain aminoguanidine hydrochloride, and the aminoguanidine hydrochloride obtained through synthesis and dipropylidene diamine are polymerized to obtain the polymer. The specific preparation steps comprise synthesis and polymerization, wherein the dicyandiamine and the ammonia chloride are synthesized under the protection of inert nitrogen at the temperature of 150 to 200DEG C to obtain the aminoguanidine hydrochloride; the aminoguanidine hydrochloride obtained through the synthesis and the dipropylidene diamine are put into a polymerization kettle to react at the temperature gradually raised, the specific temperatures are as follows: the temperature of 100 to 130DEG C is maintained for one hour, the temperature of 130 to 150DEG C is maintained for one hour, the temperature of 150 to 180DEG C is maintained for one hour, and the temperature of 180 to 210DEG C is maintained for one hour; then 1% to 3% of a terminating agent is added to terminate the reaction, and a polyhexamethylene guanidine polymer is obtained. When the present invention is used as a raw material for a bactericide, the obtained bactericide which is nontoxic has no irritation to the skin, the mucous membranes or the eyes and does not perform carcinogenicity action nor teratogenicity action, and therefore, the obtained bactericide can be safely and effectively applied to daily disinfection, sanitary accessory disinfection, environment disinfection, etc.
Description
Technical field
The present invention relates to the polymkeric substance in the chemical field, specifically a kind of preparation method of new multi-purpose high molecular polymer-polyhexamethylene guanidine.
Background technology
Be used for sterilization, disinfectant material in the prior art, stronger toxicity is all arranged, pungency, corrodibility, poor stability need promptly be joined i.e. usefulness simultaneously, and some is also inflammable and explosive, and majority has bigger side effect.The sterilization expert proposes the requirement to the optimum chemical sterilizing agent: fungicidal spectrum is wide; Effective concentration is low; Speed of action is fast; Stable in properties; Soluble in water; Can use at normal temperatures; Antibacterial for a long time, have no side effect; Non-corrosiveness; Colourless, tasteless, nothing is smelt; Toxicity is low; Do not fire, not quick-fried, safe in utilization; Moderate; Convenient transportation.According to these experts practice for many years, conclusion is that the sterilizing agent that uses at present all can not satisfy above requirement fully.
Summary of the invention
The preparation method of a kind of new multi-purpose high molecular polymer of providing at the deficiencies in the prior art is provided, and this polymkeric substance has purposes extremely widely in industrial, agriculture, medical and daily life.
At first it can brute force kill each bacterioid, is used as material of germicide, and that the gained sterilant has is nontoxic, harmless, non-stimulated, the burn into performance of not bleaching not; But be used as mould inhibitor formula leatherware and have the antifungal effect.In petroleum industry, can improve the efficient of tertiary oil recovery.In agricultural and aquaculture, can be widely used for, cure the disease fowl poultry, fishes and shrimps diseases prevention.Secondly it has good throwing out, in sewage disposal, both can clean water quality, but sterilization again.It in aquaculture excellent water quality amendment.
The concrete technical scheme that realizes the object of the invention is: a kind of method for preparing the polyhexamethylene guanidine polymer, characteristics are that it adopts dicyandiamide, the synthetic hydrochloric acid amido guanidine that obtains of ammonia chloride, obtain this polymkeric substance (polyhexamethylene guanidine) with synthetic hydrochloric acid amido guanidine and the dipropylenediamine polymerization that obtains again.
Above-mentioned polymkeric substance prepares according to the following steps:
(1), synthetic: under protection of nitrogen gas, temperature is 150-200 ℃ synthesizes, and obtains hydrochloric acid amido guanidine with chemical pure dicyandiamide and ammonia chloride (1: 1 mol ratio);
(2), polymerization: will synthesize the hydrochloric acid amido guanidine and six trimethylene diamines that obtain and put into polymeric kettle, and progressively heat up, and react, actual temp is: 100-130 ℃ kept one hour; 130-150 ℃ kept one hour; 150-180 ℃ kept one hour; 180-210 ℃ kept one hour, added the termination agent of 1%-3% then, and the stopping of reaction obtains the polyhexamethylene guanidine polymer.
Do material of germicide with the polymkeric substance that the present invention obtains, the gained sterilant can reach 99.99% by the killing rate to intestinal bacteria, staphylococcus aureus, Candida albicans for powerful through Shanghai preventive medicine researcher test in 2-5 minute, through LD50＞5 of toxicity detection to big white mouse, 000mg/Kg is actual nontoxic level, all non-stimulated to skin, mucous membrane, eyes, and do not have carcinogenic and the aberration inducing effect.Can be applied to daily, therapeutic medical all kinds of surface sterilizations such as daily sterilization, sanitary product sterilization, environment disinfected safely and effectively.Through stability test, still keep performance constant in three months.
Embodiment
To obtain the present invention's 1000 grams is example:
(1), synthetic: get 320 gram chemical pure dicyandiamides, 209 gram ammonia chlorides under nitrogen protection, temperature is 180 ℃ synthesizes, and obtains 450 gram hydrochloric acid amido guanidines;
(2), polymerization: will synthesize the 450 hydrochloric acid amido guanidines and 680 grams, six trimethylene diamines that obtain and put into polymeric kettle, and progressively heat up, and react, actual temp is: 120 ℃ kept one hour; 150 ℃ kept one hour; 180 ℃ kept one hour; 200 ℃ kept one hour, added 10 gram polyvinyl alcohol then and ended agent, and the stopping of reaction obtains 1000 gram polyhexamethylene guanidine polymers.
When being used as the material of germicide use, resulting polymers is dissolved in the 3000 gram water, be mixed with 25% solution and get final product.
25% solution is as the stoste of sterilant.When the preparation sterilant, can dilute 50-125 doubly (according to the use occasion difference, working concentration is higher in the severe contamination area, and in the uncontamination district, as prophylactic disinfection, then working concentration is low).
Claims (1)
1, a kind of method for preparing the polyhexamethylene guanidine polymer is characterized in that it prepares according to the following steps:
(1), synthetic: with chemical pure dicyandiamide and ammonia chloride, fill a part mixing with 1: 1 mol ratio, under protection of nitrogen gas, temperature is 150-200 ℃ synthesizes, and obtains hydrochloric acid amido guanidine;
(2), polymerization: will synthesize the hydrochloric acid amido guanidine and six trimethylene diamines that obtain and put into reactor, and progressively heat up, and react, actual temp is: 100-130 ℃ kept one hour; 130-150 ℃ kept one hour; 150-180 ℃ kept one hour; 180-210 ℃ kept one hour, added the termination agent of 1%-3% then, and the stopping of reaction obtains the polyhexamethylene guanidine polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116731 CN1239574C (en) | 2003-05-01 | 2003-05-01 | Macromolecule polymer and method for preparing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116731 CN1239574C (en) | 2003-05-01 | 2003-05-01 | Macromolecule polymer and method for preparing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1542033A CN1542033A (en) | 2004-11-03 |
| CN1239574C true CN1239574C (en) | 2006-02-01 |
Family
ID=34320462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03116731 Expired - Lifetime CN1239574C (en) | 2003-05-01 | 2003-05-01 | Macromolecule polymer and method for preparing the same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1239574C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7561778B2 (en) | 2002-05-07 | 2009-07-14 | Lg Electronics Inc. | Method for recording and managing a multi-channel stream |
| US7672567B2 (en) | 2002-06-24 | 2010-03-02 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple reproduction path video data for at least a segment of a title recorded thereon and recording and reproducing methods and apparatuses |
| US7693394B2 (en) | 2003-02-26 | 2010-04-06 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of data streams recorded thereon and recording and reproducing methods and apparatuses |
| US7769272B2 (en) | 2002-11-20 | 2010-08-03 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of at least video data recorded thereon and recording and reproducing methods and apparatuses |
| US7809775B2 (en) | 2003-02-27 | 2010-10-05 | Lg Electronics, Inc. | Recording medium having data structure for managing playback control recorded thereon and recording and reproducing methods and apparatuses |
| US7809243B2 (en) | 2002-06-24 | 2010-10-05 | Lg Electronics, Inc. | Recording medium having data structure including navigation control information for managing reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
| US7813237B2 (en) | 2002-10-14 | 2010-10-12 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple audio streams recorded thereon and recording and reproducing methods and apparatuses |
| US7835622B2 (en) | 2002-06-21 | 2010-11-16 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
| US7835623B2 (en) | 2002-06-21 | 2010-11-16 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of video data recorded thereon |
| US7848619B2 (en) | 2003-04-04 | 2010-12-07 | Lg Electronics Inc. | Recording medium having data structure for managing to resume reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245141B (en) * | 2007-02-16 | 2011-04-06 | 铜陵高聚生物科技有限公司 | Hydrochloric polyhexamethylene guanidine and preparation method thereof |
| CN101857539B (en) * | 2009-04-09 | 2013-04-17 | 宁波大学 | Method for producing adipic acid, hexamethylenediamine sulfate and polyhexamethylene (di)guanidine sulfate from nylon-66 through depolymerization |
| CN102283251B (en) * | 2011-07-04 | 2013-03-13 | 朱晓鸣 | Agricultural sterilization solution |
| CN111838171A (en) * | 2020-08-14 | 2020-10-30 | 上海黛龙生物工程科技有限公司 | Compound disinfectant and preparation method thereof |
-
2003
- 2003-05-01 CN CN 03116731 patent/CN1239574C/en not_active Expired - Lifetime
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7561778B2 (en) | 2002-05-07 | 2009-07-14 | Lg Electronics Inc. | Method for recording and managing a multi-channel stream |
| US7835623B2 (en) | 2002-06-21 | 2010-11-16 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of video data recorded thereon |
| US7835622B2 (en) | 2002-06-21 | 2010-11-16 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
| US7809243B2 (en) | 2002-06-24 | 2010-10-05 | Lg Electronics, Inc. | Recording medium having data structure including navigation control information for managing reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
| US7783159B2 (en) | 2002-06-24 | 2010-08-24 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple reproduction path video data for at least a segment of a title recorded thereon and recording and reproducing methods and apparatuses |
| US7672567B2 (en) | 2002-06-24 | 2010-03-02 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple reproduction path video data for at least a segment of a title recorded thereon and recording and reproducing methods and apparatuses |
| US7949231B2 (en) | 2002-06-24 | 2011-05-24 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple reproduction path video data recorded thereon and recording and reproducing methods and apparatuses |
| US7813237B2 (en) | 2002-10-14 | 2010-10-12 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple audio streams recorded thereon and recording and reproducing methods and apparatuses |
| US7961570B2 (en) | 2002-10-14 | 2011-06-14 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple audio streams recorded thereon and recording and reproducing methods and apparatuses |
| US7769272B2 (en) | 2002-11-20 | 2010-08-03 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of at least video data recorded thereon and recording and reproducing methods and apparatuses |
| US8831406B2 (en) | 2002-11-20 | 2014-09-09 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of at least video data recorded thereon and recording and reproducing methods and apparatuses |
| US7693394B2 (en) | 2003-02-26 | 2010-04-06 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of data streams recorded thereon and recording and reproducing methods and apparatuses |
| US7809775B2 (en) | 2003-02-27 | 2010-10-05 | Lg Electronics, Inc. | Recording medium having data structure for managing playback control recorded thereon and recording and reproducing methods and apparatuses |
| US7848619B2 (en) | 2003-04-04 | 2010-12-07 | Lg Electronics Inc. | Recording medium having data structure for managing to resume reproduction of video data recorded thereon and recording and reproducing methods and apparatuses |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1542033A (en) | 2004-11-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1239574C (en) | Macromolecule polymer and method for preparing the same | |
| CA2319342C (en) | Biocidal compositions for treating water | |
| US6436445B1 (en) | Antimicrobial and antiviral compositions containing an oxidizing species | |
| JP5065244B2 (en) | Acidified chlorite disinfectant composition having an olefin stabilizer | |
| CN101731257B (en) | Polyhexamethylene guanidine compound disinfectant and preparation method | |
| US6663902B1 (en) | Method and composition for the generation of chlorine dioxide using Iodo-Compounds, and methods of use | |
| CN101933521A (en) | Preparation and application thereof of sterilization composition | |
| CN101642449B (en) | Skin mucous membrane disinfectants and preparation method thereof | |
| JPH10505117A (en) | Ionene polymers containing biologically active anions | |
| PL206314B1 (en) | Aqueous solution of non-colloidal silicic acid and boric acid | |
| WO2008118940A2 (en) | Compositions and methods to control the growth of microorganisms in aqueous systems | |
| US4018592A (en) | Method of controlling the growth of algae | |
| CN102090413A (en) | Preparation and application of compound disinfectant | |
| CN1215161C (en) | Chitin betaine surfactant composition and its preparation and agent | |
| WO1990009405A1 (en) | Ammonium compound, composition containing it and desinfection method | |
| CN102302033A (en) | Preparation and application of compounded disinfection atomization agent | |
| AU2004294286B2 (en) | Antimicrobial compositions comprising polymeric stabilizers | |
| US5019380A (en) | Novel antimicrobial compositions and process for preparing the same | |
| CN1556046A (en) | Synergism type chlorine dioxide bactericide and its manufacturing method and use in aquatic culture | |
| CN104650352A (en) | Poly-hexamethylene biguanide hydrochloride sterilizing and disinfecting agent | |
| CN106832267B (en) | A kind of guanidine copolymer and preparation method thereof | |
| MXPA96000116A (en) | Biocidal composition stable in storage and procedure to produce the same. | |
| CN107326463B (en) | A kind of preparation method of polymethylene guanidine modification PVC anti-bacterial fibre | |
| CN112335655A (en) | Environment-friendly compound bactericide suitable for high-temperature and alkaline environment and preparation method thereof | |
| RU2022564C1 (en) | Disinfection agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20060201 |
|
| CX01 | Expiry of patent term |