CN1268608C - Process for preparing n-dodecylguanidineacetate - Google Patents
Process for preparing n-dodecylguanidineacetate Download PDFInfo
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- CN1268608C CN1268608C CN 200410054040 CN200410054040A CN1268608C CN 1268608 C CN1268608 C CN 1268608C CN 200410054040 CN200410054040 CN 200410054040 CN 200410054040 A CN200410054040 A CN 200410054040A CN 1268608 C CN1268608 C CN 1268608C
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- dodine
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Abstract
The present invention discloses a method for preparing n-dodecylguanidine monoacetate by using urea as raw material. The method has the advantages of low production cost and high product purity and is suitable for industrial large-scale production. The n-dodecylguanidine monoacetate can be used as an agricultural chemical and used for fruit trees and agriculture crops to prevent leaves from curling, fruits from suffering from injurious insects, etc.; therefore, the n-dodecylguanidine monoacetate belongs to a low toxicity germicidal agent. Besides, the n-dodecylguanidine monoacetate can be also used as a sterilizing agent for treating industrial waste water, used as a washing agent for washing and nursing hairs and cleaning mechanical devices, used as a seed treatment agent, a sterilization treatment agent for appliances for women and children and food wrappers, etc.
Description
Technical field
The present invention relates to chemical field, especially, relating to a kind of is the method for the positive dodine of feedstock production with urea.
Background technology
A positive dodine (1-Dodecylguanidineacetate) is commonly called as dodine (dodine), is 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 is the positive dodine method of feedstock production with urea.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of a positive 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 methyl alcohol, ethanol, propyl alcohol or butanol solution;
(3) separating and filtering;
(4) building-up reactions: under 0～60 ℃ of temperature, amino dodecane, Glacial acetic acid and neutralization filtrate reaction are obtained a positive dodine solution;
(5) freezing and crystallizing, separation oven dry obtain product.
Further, in the step (1), the mol ratio of described methyl-sulfate and urea is 2: 1～2: 3; In the step (2), described alkali metal hydroxide is sodium hydroxide or potassium hydroxide; In the step (5), described freezing and crystallizing temperature is-20～15 ℃, and the described freezing and crystallizing time is 1～40 hour, and described bake out temperature is 40～120 ℃.
The present invention has following technique effect: prepare a positive 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.The positive dodine of synthetic can be used as agricultural chemicals, 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; 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 the positive dodine solution that obtains freezing and crystallizing 1～40 hour under-20～15 ℃ of temperature, filter, filtrate dried under 40～120 ℃ of temperature obtain the positive dodine of product, 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 the positive dodine solution that obtains freezing and crystallizing 1～40 hour under-20～15 ℃ of temperature, filter, filtrate dried under 40～120 ℃ of temperature obtain the positive dodine of product, 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 (5)
- 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 methyl alcohol, ethanol, propyl alcohol or butanol 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 alkali metal hydroxide is sodium hydroxide or potassium hydroxide.
- 4. 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.
- 5. the preparation method of just according to claim 1-dodine is characterized in that, in the step (5), 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 CN1629138A (en) | 2005-06-22 |
| CN1268608C true CN1268608C (en) | 2006-08-09 |
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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) |
Families Citing this family (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 |
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2004
- 2004-08-24 CN CN 200410054040 patent/CN1268608C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1629138A (en) | 2005-06-22 |
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Granted publication date: 20060809 Termination date: 20100824 |