CN103539706A

CN103539706A - Alkyl guanidine salt and preparation method thereof

Info

Publication number: CN103539706A
Application number: CN201310519839.1A
Authority: CN
Inventors: 不公告发明人
Original assignee: Individual
Current assignee: Individual
Priority date: 2013-10-30
Filing date: 2013-10-30
Publication date: 2014-01-29

Abstract

The invention relates to an alkyl guanidine salt and a preparation method thereof. Mono-alkyl-substituted ammonia reacts with a water solution of acid under the temperature condition of 0-100 DEG C, so as to generate a salt of the mono-alkyl-substituted ammonia, and then the salt reacts with cyanamide under the temperature condition of 10-100 DEG C. Thus, the product alkyl guanidine salt is obtained.

Description

A kind of alkyl guanidine salt and preparation method thereof

Technical field

The invention belongs to chemical and manufacture field, be specifically related to a kind of superficiality agent, a kind of alkyl guanidine salt and preparation method thereof.

Background technology

Chain alkyl guanidinesalt is due to its superior performance, in fields such as the sterilization in each field and textile auxiliary agenies, can have been widely used, and according to purposes, uses the primary amine of different alkyl, can in all kinds of purposes, have excellent performance;

The monoalkyl replacement ammonia salts solution that synthetic employing monoalkyl replacement ammonia and aqueous acid are synthetic and amido cyanogen are 10-100 ℃ of condensation, and reaction is easily carried out, and nontoxic, is a desirable preparation method.

Summary of the invention

Goal of the invention: problem to be solved by this invention is to provide a kind of synthetic method of novel organic raw material, a kind of synthetic method of alkyl guanidine salt;

Specifically by following processing step, realize the present invention:

(1) in reactor, drop into 1-10mol aqueous acid and 1-10mol monoalkyl and replace ammonia, under 0-100 ℃ of temperature condition, neutralization reaction is to PH=6.5-7;

(2) again in reactor, drop into cyanamide, be then warming up to 10-100 ℃ of condensation reaction 5-200 minute, clarify to material;

(3) to above-mentioned (2), add acid to PH=2-7, obtain alkyl guanidine salt finished product;

Described a kind of alkyl guanidine salt and preparation method thereof, its main raw material is: monoalkyl replaces ammonia, cyanamide, aqueous acid, and monoalkyl wherein replaces ammonia and refers to: C number is that 6,8,9,10,11,13,14,15,16,17,18 pure monoalkyl replaces ammonia or replaces the mixture of ammonia with other monoalkyl;

Described a kind of alkyl guanidine salt and preparation method thereof, the mol ratio that its synthesis material monoalkyl replaces ammonia, cyanamide, acid is: 1-10: 1-10:1-20;

Described a kind of alkyl guanidine salt and preparation method thereof, described in it, aqueous acid can be aqueous hydrochloric acid, aqueous acetic acid, aqueous formic acid;

Described a kind of alkyl guanidine salt and preparation method thereof, described in it, the neutralization reaction temperature of monoalkyl replacement ammonia is 0-100 ℃, condensation temp is 10-100 ℃;

Described a kind of alkyl guanidine salt and preparation method thereof, the alkyl in its finished product structure can be normal chain alkyl or isomery alkyl;

Described a kind of alkyl guanidine salt and preparation method thereof, described in it, the finished product pH value of alkyl guanidine salt is at 2-7;

Described a kind of alkyl guanidine salt and preparation method thereof, its synthesis step and processing condition are as above-mentioned (1)-(3) bar;

Effect of the present invention and benefit are:

(1) aspect synthetic technology: favorable reproducibility, process stabilizing, energy consumption is low, and the ammonia that can use the monoalkyl of different carbon numbers to replace according to purposes is obtained the product of different performance, selects flexibly;

(2) aspect economic benefit: product cost performance is high, sterilization is 2-3 times of alkyl benzyl ammonium chloride, in printing and dyeing as retarding agent be commercially available retarding agent 2-4 doubly, and energy consumption is better than contrast product with synthesis technique operability, economic benefit is much better than the serial product of alkyl benzyl ammonium chloride;

(3) at quality product aspect of performance: because product purity is high, reach more than 99%, effective constituent can be allocated as required, simple to operate, be beneficial to the direct use of Subscriber Unit, improved production efficiency;

Embodiment, below by embodiment, further illustrates the present invention, and this embodiment is only the present invention is described and never limits the present invention:

Embodiment 1

In reactor, drop into 20% aqueous hydrochloric acid 130-200 gram, temperature control is at 0-100 ℃, slowly add 97% single octadecyl to replace ammonia 250-280 gram, be stirred to PH to PH=6.5-7, in reactor, drop into the about 45-55 gram of 97% cyanamide again, be then warming up to 10-100 ℃ of condensation reaction 5-200 minute, then to adding aqueous hydrochloric acid in still, to material, clarify to PH=2-7, obtain finished product octadecyl guanidine hydrochloride;

Embodiment 2

In reactor, drop into 50% aqueous acetic acid 50-80 gram, temperature control is at 0-100 ℃, slowly add 97% single 12/14 mixed alkyls to replace ammonia 160-220 gram, be stirred to PH to PH=6.5-7, in reactor, drop into the about 45-55 gram of 97% cyanamide again, be then warming up to 10-100 ℃ of condensation reaction 5-200 minute, then to adding aqueous acetic acid in still, to material, clarify to PH=2-7, obtain finished product 12/tetradecyl guanidine acetate;

Embodiment 3

In reactor, drop into the about 90-120 gram of 50% aqueous formic acid, temperature control is at 0-100 ℃, slowly add 97% single octyl to replace ammonia 130-150 gram, be stirred to PH to PH=6.5-7, in reactor, drop into the about 45-55 gram of 97% cyanamide again, be then warming up to 10-100 ℃ of condensation reaction 5-200 minute, then to adding aqueous formic acid in still, to material, clarify to PH=2-7, obtain finished product octyl guanidine formate.

Claims

1. alkyl guanidine salt and preparation method thereof, is characterized in that comprising the steps and processing condition:

(1) in reactor, drop into the ammonia that 1-10mol aqueous acid and 1-10mol monoalkyl replace, under 0-100 ℃ of temperature condition, neutralization reaction is to PH=6.5-7;

(3) to above-mentioned (2), add acid to PH=2-7, obtain alkyl guanidine salt finished product.

2. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, it is characterized in that main raw material is: monoalkyl replaces ammonia, cyanamide, aqueous acid, and monoalkyl wherein replaces ammonia and refers to: C number is that 6,8,9,10,11,13,14,15,16,17,18 pure monoalkyl replaces ammonia or replaces the mixture of ammonia with other monoalkyl.

3. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: the mol ratio that synthesis material monoalkyl replaces ammonia, cyanamide, acid is: 1-10: 1-10:1-20.

4. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: described aqueous acid can be aqueous hydrochloric acid, aqueous acetic acid, aqueous formic acid.

5. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: the neutralization reaction temperature that described monoalkyl replaces ammonia is 0-100 ℃, and condensation temp is 10-100 ℃.

6. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: the alkyl in finished product structure can be normal chain alkyl or isomery alkyl.

7. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: the finished product pH value of described alkyl guanidine salt is at 2-7.

8. a kind of alkyl guanidine salt according to claim 1 and preparation method thereof, is characterized in that: it is characterized in that synthesis step and processing condition are as above-mentioned (1)-(3) bar.