CN1629138A - Process for preparing n-dodecylguanidineacetate - Google Patents
Process for preparing n-dodecylguanidineacetate Download PDFInfo
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- CN1629138A CN1629138A CN 200410054040 CN200410054040A CN1629138A CN 1629138 A CN1629138 A CN 1629138A CN 200410054040 CN200410054040 CN 200410054040 CN 200410054040 A CN200410054040 A CN 200410054040A CN 1629138 A CN1629138 A CN 1629138A
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- dodine
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Abstract
The invention provides a process for preparing n-dodecylguanidineacetate by using urea as raw material, wherein the process has the advantages of low cost of production and high product purity. The preparred n-dodecylguanidineacetate can be used as low toxity germicide, disinfectant germicide, washing agent, seed additive and sterilization agent.
Description
Technical field
The present invention relates to chemical field, especially, relate to a kind of with urea be feedstock production just-method of dodine.
Background technology
Just-and dodine (1-Dodecylguanidineacetate), be commonly called as dodine (dodine), be a kind of broad-spectrum tensio-active agent.It is used as agricultural chemicals in some countries at first, is used for fruit tree and farm crop, prevents that the incrustation of leaf rolling, fruit is infested etc., belongs to the lower toxicity sterilant.Along with the further investigation to this compound, its purposes also more and more widely can also be used as disinfectant except that using used as pesticides; Be used for industrial water conditioning agent; Washing composition be can also be used as, hair conditioning, wash machine equipment are used to wash; As disinfection treatment agent of seed treatment agent and women and children's articles for use and food wrapper etc.
The currently known methods of preparation dodine is to adopt cyanamide and amino dodecane and Glacial acetic acid reaction to obtain.Describe in the patent (DE 3248115): react in a kind of inert solvent by amino dodecane and cyanamide and acetic acid and produce dodine, the dodine and the amino dodecane of residual mother liquor are selectively separated out, (US 3004065 at United States Patent (USP), US 3,383,408, US1,257,270) also carried out same description in.But cyanamide character is active, is difficult for stably stored, uses the high energy consumption lime nitrogen to make raw material in the production, and skin contact causes strong allergy, so be subjected to certain restriction in suitability for industrialized production.
The present invention is to be that starting raw material prepares acetic acid 12 guanidines by the raw material urea that is easy to get.
Summary of the invention
The object of the present invention is to provide a kind of with urea be feedstock production just-the dodine method.
The objective of the invention is to be achieved through the following technical solutions: just a kind of preparation method of-dodine, it is characterized in that, may further comprise the steps:
(1) condensation reaction: in 60～110 ℃ of temperature ranges,, obtain oxygen methyl-isourea salt with methyl-sulfate and urea condensation;
(2) neutralization reaction: under 0～50 ℃ of temperature, condensated liquid and alkali metal hydroxide are neutralized in low-alcohol solution;
(3) separating and filtering;
(4) building-up reactions: under 0～60 ℃ of temperature, amino dodecane, Glacial acetic acid and neutralization filtrate reaction are just being obtained-dodine solution;
(5) freezing and crystallizing, separation oven dry obtain product.
The present invention has following technique effect: just preparing-dodine with method provided by the invention, manufacturing cost is low, and the product purity height is simple to operate, and is suitable for industrial mass production.Synthetic just-dodine can be used as agricultural chemicals, is used for fruit tree and farm crop, prevents that leaf rolling, fruit incrustation are infested etc., belongs to the lower toxicity sterilant; Can also be used as disinfectant, be used for industrial water conditioning agent; As washing composition, be used to wash hair conditioning, wash machine equipment; Be used as the disinfection treatment agent of seed treatment agent and women and children's articles for use and food wrapper etc.
Embodiment
Describe the specific embodiment of the invention below in detail.
Embodiment 1
2 parts of methyl-sulfates and 1 part of urea carefully heat, in 60～110 ℃ of temperature ranges, obtain oxygen methyl-isourea salt condensated liquid. condensated liquid is reacted with 10 parts of lower alcohols and 1 part of potassium hydroxide under 0～50 ℃ of temperature, separating and filtering, then filtrate is reacted with 1 part of amino dodecane and 1 part of Glacial acetic acid under 0～60 ℃ of temperature, with obtain just-dodine solution freezing and crystallizing 1～40 hour under-20～15 ℃ of temperature, filter, with filtrate under 40～120 ℃ of temperature, dry obtain product just-dodine, product purity reaches 98%.
Embodiment 2
2 parts of methyl-sulfates and 3 parts of urea carefully heat, in 60～110 ℃ of temperature ranges, obtain oxygen methyl-isourea salt condensated liquid. condensated liquid is reacted with 10 parts of lower alcohols and 1 part of sodium hydroxide under 0～50 ℃ of temperature, separating and filtering, then filtrate is reacted with 1 part of amino dodecane and 1 part of Glacial acetic acid under 0～60 ℃ of temperature, with obtain just-dodine solution freezing and crystallizing 1～40 hour under-20～15 ℃ of temperature, filter, with filtrate under 40～120 ℃ of temperature, dry obtain product just-dodine, product purity reaches 98%.
Among the embodiment, lower alcohol can be ethanol, methyl alcohol, propyl alcohol or butanols.The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (6)
- One kind just-preparation method of dodine, it is characterized in that, may further comprise the steps:(1) condensation reaction: in 60～110 ℃ of temperature ranges,, obtain oxygen methyl-isourea salt with methyl-sulfate and urea condensation.(2) neutralization reaction: under 0～50 ℃ of temperature, condensated liquid and alkali metal hydroxide are neutralized in low-alcohol solution.(3) separating and filtering.(4) building-up reactions: under 0～60 ℃ of temperature, amino dodecane, Glacial acetic acid and neutralization filtrate reaction are just being obtained-dodine solution.(5) freezing and crystallizing, separation oven dry obtain product.
- 2. the preparation method of just according to claim 1-dodine is characterized in that, in the step (1), the mol ratio of described methyl-sulfate and urea is 2: 1～2: 3.
- 3. the preparation method of just according to claim 1-dodine is characterized in that, in the step (2), described lower alcohol is methyl alcohol, ethanol, propyl alcohol or butanols.
- 4. the preparation method of just according to claim 1-dodine is characterized in that, in the step (2), described alkali metal hydroxide is sodium hydroxide or potassium hydroxide.
- 5. the preparation method of just according to claim 1-dodine is characterized in that, in the step (5), described freezing and crystallizing temperature is-20～15 ℃, and the described freezing and crystallizing time is 1～40 hour.
- 6. the preparation method of just according to claim 2-dodine is characterized in that, described bake out temperature is 40～120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410054040 CN1268608C (en) | 2004-08-24 | 2004-08-24 | Process for preparing n-dodecylguanidineacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410054040 CN1268608C (en) | 2004-08-24 | 2004-08-24 | Process for preparing n-dodecylguanidineacetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1629138A true CN1629138A (en) | 2005-06-22 |
| CN1268608C CN1268608C (en) | 2006-08-09 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410054040 Expired - Fee Related CN1268608C (en) | 2004-08-24 | 2004-08-24 | Process for preparing n-dodecylguanidineacetate |
Country Status (1)
| Country | Link |
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| CN (1) | CN1268608C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104472526A (en) * | 2014-11-25 | 2015-04-01 | 苏州佑君环境科技有限公司 | Lauryl guanidine acetate bactericide for water treatment and preparation method thereof |
| CN106968133A (en) * | 2017-04-18 | 2017-07-21 | 邱雪平 | A kind of wrapping paper bactericide and its application method |
| CN107304175A (en) * | 2016-04-21 | 2017-10-31 | 上海生农生化制品有限公司 | A kind of synthetic method of dodine |
-
2004
- 2004-08-24 CN CN 200410054040 patent/CN1268608C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104472526A (en) * | 2014-11-25 | 2015-04-01 | 苏州佑君环境科技有限公司 | Lauryl guanidine acetate bactericide for water treatment and preparation method thereof |
| CN107304175A (en) * | 2016-04-21 | 2017-10-31 | 上海生农生化制品有限公司 | A kind of synthetic method of dodine |
| CN106968133A (en) * | 2017-04-18 | 2017-07-21 | 邱雪平 | A kind of wrapping paper bactericide and its application method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1268608C (en) | 2006-08-09 |
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Granted publication date: 20060809 Termination date: 20100824 |