CN1239574C - Macromolecule polymer and method for preparing the same - Google Patents
Macromolecule polymer and method for preparing the same Download PDFInfo
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- 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
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- 229920000642 polymer Polymers 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 4
- 229920002521 macromolecule Polymers 0.000 title 1
- -1 polyhexamethylene guanidine Polymers 0.000 claims abstract description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 10
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 7
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 7
- 125000003368 amide group Chemical group 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 10
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 210000004400 mucous membrane Anatomy 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- UBDZFAGVPPMTIT-UHFFFAOYSA-N 2-aminoguanidine;hydron;chloride Chemical compound [Cl-].NC(N)=N[NH3+] UBDZFAGVPPMTIT-UHFFFAOYSA-N 0.000 abstract 4
- 239000003899 bactericide agent Substances 0.000 abstract 3
- 230000015572 biosynthetic process Effects 0.000 abstract 3
- 238000003786 synthesis reaction Methods 0.000 abstract 3
- 150000004985 diamines Chemical class 0.000 abstract 2
- 206010007269 Carcinogenicity Diseases 0.000 abstract 1
- 206010043275 Teratogenicity Diseases 0.000 abstract 1
- 230000007670 carcinogenicity Effects 0.000 abstract 1
- 231100000260 carcinogenicity Toxicity 0.000 abstract 1
- 230000007794 irritation Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 231100000211 teratogenicity Toxicity 0.000 abstract 1
- 230000001954 sterilising effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000002070 germicidal effect Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 238000009360 aquaculture Methods 0.000 description 2
- 244000144974 aquaculture Species 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000003206 sterilizing agent Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000143060 Americamysis bahia Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000069 prophylactic effect Effects 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (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
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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 (11)
| 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 |
| US7606463B2 (en) | 2003-02-24 | 2009-10-20 | Lg Electronics, Inc. | Recording medium having data structure for managing playback control and recording and reproducing methods and apparatuses |
| US7606465B2 (en) | 2002-06-24 | 2009-10-20 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple title video data recorded thereon and recording and reproducing methods and apparatuses |
| US7620301B2 (en) | 2003-04-04 | 2009-11-17 | Lg Electronics Inc. | System and method for resuming playback |
| 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 |
| 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 |
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 (17)
| 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 |
| 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 |
| 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 |
| 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 |
| US7606465B2 (en) | 2002-06-24 | 2009-10-20 | Lg Electronics Inc. | Recording medium having data structure for managing reproduction of multiple title 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 |
| 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 |
| US7606463B2 (en) | 2003-02-24 | 2009-10-20 | Lg Electronics, Inc. | Recording medium having data structure for managing playback control 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 |
| US7620301B2 (en) | 2003-04-04 | 2009-11-17 | Lg Electronics Inc. | System and method for resuming playback |
| 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 |
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