CN1390876A - Polyhexaethylene. guanidine as raw material of bactericide and its preparing process - Google Patents
Polyhexaethylene. guanidine as raw material of bactericide and its preparing process Download PDFInfo
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- CN1390876A CN1390876A CN 02135317 CN02135317A CN1390876A CN 1390876 A CN1390876 A CN 1390876A CN 02135317 CN02135317 CN 02135317 CN 02135317 A CN02135317 A CN 02135317A CN 1390876 A CN1390876 A CN 1390876A
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- germicide
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- bactericide
- hexamethylene
- diamine
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- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
A polyhexamethylene guanidine hydrochloride as the raw material of bactericide contains imidourea hydrochloride (42-44 wt.%), hexamethylenediamine (52-54), polyethanediol (3-5), toluene-4-sulfonic acid (0.005-0.009). It can be used as bactericide after diluted with distilled water by 200-1000 times. Its advantages are no pollution, broad spectrum, and high effect and stability.
Description
The present invention relates to a kind of material of germicide Polyhaxemethylenguanidine Hydrochloride and preparation method thereof.The sterilization and disinfection that is used for mucocutaneous in textile industry, agricultural, food service industry, livestock industry, the hospital, body surface and daily life.
Existing sterilant kind is a lot, and bactericidal property differs, and the branch of high, medium and low effect is arranged.The effective concentration of efficient germicide is also high often, and cost value is also high.And existing sterilant poor stability, toxic, corrodibility, irritating smell also have certain pollution to environment.Therefore, people wish to have always a kind of can sterilization the sterilant of safety and stability again.
The object of the present invention is to provide a kind ofly can overcome the insufficient sterilant of existing procucts, belong to nontoxic, colourless, do not have smell, the free of contamination food grade products of non-stimulated, no burn into, have efficiently, characteristics such as wide spectrum, good stability.
Main points of the present invention are to select suitable component, and carry out rational temperature control, a kind of material of germicide Polyhaxemethylenguanidine Hydrochloride that forms through polyreaction.
The prescription following (component and weight percent % thereof) that the present invention selects:
Salt acid imide urea 42～44
Hexamethylene-diamine 52～54
Polyoxyethylene glycol 3～5
Toluene-4-sulfonic acid 0.005～0.009
Salt acid imide urea and hexamethylene-diamine are as main sterilization component, guanidine radicals in this component has very high activity in polyreaction, make polymkeric substance be positive polarity, so it is adsorbed to be easy to be electronegative each bacterioid usually, thereby the splitting function that has suppressed bacterium, make bacterium lose reproductive performance, add that the film of polymer formation has stopped up the respiration channel of microorganism, is choked to death microorganism rapidly.
The molecular formula of Polyhaxemethylenguanidine Hydrochloride of the present invention is: (C
7H
16N
3Cl)
n
The structural formula of Polyhaxemethylenguanidine Hydrochloride of the present invention is:
The preparation method of product of the present invention is:
Salt acid imide urea, hexamethylene-diamine are added reactor heat and stir, add toluene-4-sulfonic acid when temperature of reaction kettle rises to 100 ℃.After reinforced, progressively be warming up to 100 ℃～150 ℃ maintenance effects 0～4 hour, add polyoxyethylene glycol after being warming up to 150 ℃, progressively be warming up to 180 ℃ of maintenance effects-1 hour.After reaction finishes, draw effective active components and be 100% faint yellow solid.
Making sterilant after 200～10000 times of the product adding distil water of the present invention dilutions compares with existing sterilant and have the following advantages: (1) is colourless, tasteless, sterilization effect is remarkable, through experiment, this product is to intestinal bacteria, streptococcus aureus, Candida albicans, gonococcus, Penicillium notatum, aspergillus tubigensis, mixing mould, Salmonellas etc., with bacteria concentration 10
6/ ml bacterium is counted meter, and 1: 2000 extent of dilution effect 5 minutes, sterilizing rate can reach 100%.(2) be specially adapted to the sterilization of skin in the hospital, mucous membrane, body surface, the sterilization of textile industry, agricultural, food service industry, livestock industry and daily life etc.(3) this product is a high molecular polymer, and chemical property is very stable, after testing, the extent of dilution at 1: 2000, in 54 ℃ of two week, effective ingredient rate of descent＜3%, 37 ℃ three months effective ingredient rate of descent＜4%, room temperature was placed 1 year, and effective ingredient descends＜6%.(4) at 1: 200 extent of dilution, LD
50Greater than the nontoxic level in the true border of 5000mg/kgBW; Cumulative toxicity test is weak cumulative toxicity, cumulative coefficient K＞5; Extent of dilution eye irritant test integration at 1: 400 is 3.0 minutes, belongs to nonirritant; The acute skin irritation test integration is 0 minute, belongs to nonirritant; The mouse polychromatic erythrocytes micronucleus test is negative, no mutagenicity; The sperm malformation test result is negative.(5) non-corrosiveness does not all have corrosion to metal, rubber, plastics, cloth etc.(6) can neutralize fully with soap class neutralizing agent, neutralized reaction product does not have bactericidal property, environmentally safe.
The present invention is described in further detail below in conjunction with embodiment:
Be configured according to the preparation method according to following table institute column data (weight percent %):
| Salt acid imide urea | Hexamethylene-diamine | Polyoxyethylene glycol | Toluene-4-sulfonic acid | |
| Embodiment 1 | ??43.1782 | ????52.4453 | ??4.3704 | ????0.0061 |
| Embodiment 2 | ??43.5581 | ????52.9068 | ??3.5271 | ????0.008 |
| Embodiment 3 | ??43.4146 | ????52.7325 | ??3.8459 | ????0.007 |
Component in the above-mentioned data sheet is added in the reactor by the preparation method, react a program after the discharging packing get final product.
Claims (3)
1. material of germicide Polyhaxemethylenguanidine Hydrochloride is characterized in that having following prescription (component and weight percent % thereof):
Salt acid imide urea 42～44
Hexamethylene-diamine 52～54
Polyoxyethylene glycol 3～5
Toluene-4-sulfonic acid 0.005～0.009
2. material of germicide Polyhaxemethylenguanidine Hydrochloride according to claim 1, its structural formula is:
3. according to the preparation method of claim 1,2 described material of germicide Polyhaxemethylenguanidine Hydrochlorides, it is characterized in that:
Salt acid imide urea, hexamethylene-diamine are added reactor heat and stir, add toluene-4-sulfonic acid when temperature of reaction kettle rises to 100 ℃.After reinforced, progressively be warming up to 100 ℃～150 ℃ maintenance effects 0～4 hour, add polyoxyethylene glycol after being warming up to 150 ℃, progressively be warming up to 180 ℃ of maintenance effects 0～1 hour.After reaction finishes, draw effective active components and be 100% faint yellow solid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135317 CN1390876A (en) | 2002-07-26 | 2002-07-26 | Polyhexaethylene. guanidine as raw material of bactericide and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02135317 CN1390876A (en) | 2002-07-26 | 2002-07-26 | Polyhexaethylene. guanidine as raw material of bactericide and its preparing process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1390876A true CN1390876A (en) | 2003-01-15 |
Family
ID=4748130
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02135317 Pending CN1390876A (en) | 2002-07-26 | 2002-07-26 | Polyhexaethylene. guanidine as raw material of bactericide and its preparing process |
Country Status (1)
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| CN (1) | CN1390876A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100444755C (en) * | 2006-07-05 | 2008-12-24 | 刘青华 | Method for prolonging aquatic product cold storage freshness preservation time using sterilizing agent |
| CN101962442A (en) * | 2009-07-21 | 2011-02-02 | 铜陵高聚生物科技有限公司 | Method for preparing polyhexamethylene biguanidine hydrochloride |
| WO2012062001A1 (en) * | 2010-11-14 | 2012-05-18 | 中国科学院华南植物园 | Use of polyhexamethylene guanidine hydrochloride as preservative for preventing and controlling citrus sour rot and its application |
| CN105820333A (en) * | 2016-04-26 | 2016-08-03 | 湖南雪天精细化工股份有限公司 | Preparation method of polyhexamethyleneguanidine hydrochloride |
| CN106087087A (en) * | 2016-06-01 | 2016-11-09 | 恒天纤维集团有限公司 | Antibacterial regenerated celulose fibre and preparation method thereof |
| CN107868023A (en) * | 2016-09-22 | 2018-04-03 | 中国石油化学工业开发股份有限公司 | Biguanide phosphate synthesis method and antibacterial agent |
-
2002
- 2002-07-26 CN CN 02135317 patent/CN1390876A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100444755C (en) * | 2006-07-05 | 2008-12-24 | 刘青华 | Method for prolonging aquatic product cold storage freshness preservation time using sterilizing agent |
| CN101962442A (en) * | 2009-07-21 | 2011-02-02 | 铜陵高聚生物科技有限公司 | Method for preparing polyhexamethylene biguanidine hydrochloride |
| WO2012062001A1 (en) * | 2010-11-14 | 2012-05-18 | 中国科学院华南植物园 | Use of polyhexamethylene guanidine hydrochloride as preservative for preventing and controlling citrus sour rot and its application |
| US9192162B2 (en) | 2010-11-14 | 2015-11-24 | South China Botanical Garden, Chinese Academy Of Sciences | Use of polyhexamethylene guanidine hydrochloride as preservative to control citrus sour rot and its application |
| CN105820333A (en) * | 2016-04-26 | 2016-08-03 | 湖南雪天精细化工股份有限公司 | Preparation method of polyhexamethyleneguanidine hydrochloride |
| CN105820333B (en) * | 2016-04-26 | 2018-04-20 | 湖南雪天精细化工股份有限公司 | A kind of preparation method of Polyhaxemethylenguanidine Hydrochloride |
| CN106087087A (en) * | 2016-06-01 | 2016-11-09 | 恒天纤维集团有限公司 | Antibacterial regenerated celulose fibre and preparation method thereof |
| CN106087087B (en) * | 2016-06-01 | 2018-02-23 | 恒天纤维集团有限公司 | Antibacterial regenerated celulose fibre and preparation method thereof |
| CN107868023A (en) * | 2016-09-22 | 2018-04-03 | 中国石油化学工业开发股份有限公司 | Biguanide phosphate synthesis method and antibacterial agent |
| TWI626229B (en) * | 2016-09-22 | 2018-06-11 | 中國石油化學工業開發股份有限公司 | Synthesis of biguanid phosphate and bactericide |
| CN107868023B (en) * | 2016-09-22 | 2020-05-08 | 中国石油化学工业开发股份有限公司 | Biguanide phosphate synthesis method and antibacterial agent |
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