CN101033202A - Organic acid stabilizer and preparation of its percarbonateamide - Google Patents

Abstract

This invention relates to a fine chemical product of percarbonamide, a crystal addition compound of hydrogen peroxide and urea, the outlook of which is white crystal powder , the theory active oxygen is 17.02%, and easy to be solved in water and the solution has the performance of hydrogen peroxide and urea liquor having good stability, slow releasing of oxygen and is effective for a long time.

Description

The preparation of organic acid stablizer and percarbamide thereof

Technical field

This invention relates to the synthetic method of percarbamide and the screening of new stabilizer thereof.This synthesis method route is succinct, simple to operate, productive rate is high, pollution-free, and waste liquid can be recycled.

Background technology

Percarbamide is a kind of fine chemistry industry product innovation, and it is the crystal adducts of hydrogen peroxide and urea, and outward appearance is a white crystalline powder, theoretical active o content is 17.02%, soluble in water, the aqueous solution has the character of hydrogen peroxide and aqueous solution of urea, good stability concurrently, release oxygen is slow, the effectiveness time is long, has widely purposes (as bleaching, sterilization, sterilize etc.), and have wide practical use.But this important fine chemical product is suddenly treated development and application in the industrial blank that also is in.At present, SPC-D complexes throughput reaches 20kt/a, and world's aggregate demand is 700kt/a, throughput does not satisfy the market requirement far away, single additive (10%-20%) with regard to washing powder, annual demand 50-100kt, and ten thousand tons of sodium percarbonate annual output less thaies.Percarbamide is a product innovation, because its advantage on performance is affirmed than SPC-D height on price.Therefore, the product that percarbamide can become a kind of update has been inevitable, but the producing country of percarbamide has only the U.S., Japan etc. now.External in recent years development and application is with the acquisition remarkable progress, though the domestic manufacturer that a lot of hydrogen peroxide and urea are arranged, the quality of stablizer directly influences the stability of product.

Summary of the invention

The synthesis technique flow process be by raw material urea and hydrogen peroxide under the condition that stablizer and coating agent exist, through synthetic, the coating crystallization is filtered, finished product is made in oven dry, the mother liquor after the filtration is preserved, and is used for next time synthetic (as shown below).Important is the screening of stablizer.

Percarbamide easily decomposes.When producing percarbamide, owing to can have a little metal ion in urea or the hydrogen peroxide. should add stablizer removing metal ion, the add-on of stablizer be urea add-on 0.5～1.0% for best, but few more good more.With the amount of stablizer when identical, 35 ℃ of reaction temperature, reaction times 30min, feed ratio are under 0.70: 1 situation, several different stabilizers are to the influence such as the following table 1 of percarbamide productive rate:

Table 1. stablizer is to the influence of reaction

	Percarbamide productive rate %0	Active o content %	Percarbamide content %	PH value
					Phenylformic acid tartrate dipotassium hydrogen phosphate	72.48 69.46 68.62	16.14 16.24 16.19	94.86 95.50 95.17	3～4 3～4 5～6

Can be found that by table 1 with hydrogen peroxide and urea synthesis percarbamide, this adduction effect can be carried out more smoothly under acidic conditions, and product stability is better, product yield is also higher.More stable dose of phenylformic acid, tartrate, dipotassium hydrogen phosphate finds that the best stabilizer is a tartrate.

Stablizer comprises: phenylformic acid, tartrate, acetate, acetone, oxysuccinic acid, citric acid, dipotassium hydrogen phosphate, Repone K etc.

Coating agent: sodium laurylsulfonate, phenylbenzimidazole sulfonic acid sodium etc.

The present invention shows, in suitable stablizer, mixes to obtain stable percarbamide with hydrogen peroxide with urea.Maximum output is higher than 70%, and active o content is higher than 16.3%.

Embodiment

Example 1

In the 500ml container, add the urea of hydrogen peroxide and respective amount, be controlled at certain temperature of reaction, after treating that urea dissolves fully, add few stable agent phenylformic acid, when question response will finish, add few coating agent sodium laurylsulfonate, stir then reflection end in 35 minutes altogether, gained solution with mixture of ice and water cooling 3-4 hour, is got white pasty state liquid, suction filtration, get the white powder crystallization, and in 30 ℃ baker, dry, promptly obtain product.Productive rate is 77.36%; Active o content 16.47%.

Example 2

Experimental technique according to example 1.Stablizer changes tartrate into.It is the same with example 1 to obtain product.Productive rate is 75.36%; Active o content 16.20%.

Example 3

Experimental technique according to example 1.Stablizer changes citric acid into.It is the same with example 1 to obtain product.Productive rate is 76.36%; Active o content 16.40%.

Claims (4)

1. one kind was synthesized phosphinylidyne ammonia preparation method, it is characterized in that carrying out in the stablizer, reacted under 35-45 ℃, condition of normal pressure.

2. in accordance with the method for claim 1, it is characterized in that using stablizer and coating agent, comprising phenylformic acid, tartrate, citric acid etc.

3. according to the described stablizer of claim 2, wherein stablizer tartrate is best.

4. it is characterized in that in accordance with the method for claim 1, should not be too high in temperature.