CN1234831C - High-powered fluorescent brightening agent and its preparing method - Google Patents

Abstract

The present invention relates to a chemical material for washing articles, more specifically to a fluorescent brightening agent (liquid 351) with high performance and a preparation method thereof. The fluorescent brightening agent is prepared from the following ingredients, in weight, more than 15 to 25% of 4, 4'-(2-ulfostyryl)-1, 1'-diphenol, 20 to 30% of nonylol polyoxyvinylether, 5 to 15% of glycerol, 15 to 30% of propanediol and 5 to 40% of deionized water. The fluorescent brightening agent has the advantages of high solubility of an effective ingredient CF-351, stable product performance, preparation and application at low temperature, low cost and no toxicity. The fluorescent brightening agent can be used as a raw material of washing powder, washing liquid, washing cream and perfumed soap.

Description

A kind of white dyes and preparation method thereof

Technical field

The present invention relates to the industrial chemicals of articles for washing, specifically a kind of white dyes (liquid 351) and preparation method thereof.

Background technology

White dyes usually uses with the form of mixtures of multiple component, because can show the performance higher than each one-component summation (whiteness) with the form of mixture; The liquid CBS-X (WO 01/12771 English 2001.2.22) that has Switzerland Ciba-Geigyg company to produce that present range of application in the world is wider, liquid CBS-X mainly is made of the water of 10～20% distyryl biphenyl base stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate, 20～50% alkoxylated fatty acid alkanol, 20～40% polyol, 0～20% diol compound and 1～50%, and it is used to improve the washing composition white appearance; Active princlple distyryl biphenyl base dithionate content among the liquid CBS-X is relatively low, and its relative price is higher.

Summary of the invention

The object of the present invention is to provide that a kind of cost is low, the white dyes that can in low temperature environment, prepare and use and preparation method thereof.

For achieving the above object, the technical scheme taked of the present invention is:

White dyes, its weight consists of:

4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl＞15～25%, polyoxyethylene nonylphenol ether 20～30%, glycerol 5～15%, propylene glycol 15～30%, deionized water 5～40%.

Described polyoxyethylene nonylphenol ether is preferably TX-4, TX-6 or TX-10; Described propylene glycol is preferably 1, the 2-propylene glycol; Described 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-weight content of biphenyl is preferably 16～22% more preferably greater than 20%; The weight content of described each component is preferably: 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl 22%, polyoxyethylene nonylphenol ether 23%, glycerol 9%, propylene glycol 18%, deionized water 28%.

The preparation method of white dyes of the present invention is as follows:

1) with after polyoxyethylene nonylphenol ether, glycerol, propylene glycol, the deionized water mixing, is warming up to 52～80 ℃;

2) adding 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl; Adopt the feed way of intermittent type or continous way, feed rate is decided according to the dissolution rate of filter cake, and the coarse filtration cake needs to add in 1.5 hours;

3) isothermal reaction is 2～6 hours, and cold water is cooled to 30 ℃ with bottom discharge; Filter elimination impurity, collect filtrate and partly be finished product.

The present invention has following advantage:

1. the solubleness height of active princlple CF-351.Have compatibleness preferably between polyoxyethylene nonylphenol ether series, propylene glycol and the glycerine that adopts among the present invention, formed solution of three and water is fine to dissolve each other and has high resolution to CF-351; Subzero polyoxyethylene nonylphenol ether series emulsifying agent under the preservation period that guarantees product reaches situation more than two months, in the reaction process of relatively-high temperature, makes the solubleness of CF-351 reach 22%; The solubleness content of CF-351 of the present invention reaches as high as 25%, and its preservation period was less than two months, but this is significant for rig-site utilization.

2. product performance are stable.The emulsifying agent that the present invention adopts has high emulsibility and solvability, is high performance polar solvent, possesses the dual good solubility to CF-351 and water; Simultaneously, the present invention adopts The optimum reaction conditions and synthetic route to guarantee that the content of CF-351 is higher in the lysate, the product shelf time is longer (standard is 60 days).

3. can in low temperature environment, prepare and use.Polyoxyethylene nonylphenol ether series its zero pour of emulsifying agent lower (in the time of 5～10 ℃, should be flowable state), be suitable in the lower environment of temperature, (for example: northern China manufacturer) using, simplified the operation sequence that white dyes prepares (having saved molten material operation) in low temperature environment, saved energy consumption, and the condensation point of products obtained therefrom also decreases.

4. cost is low.The present invention is raw materials used (for example; Emulsifying agent) price is lower, and (with employed comparing among the WO 01/12771), and be home products, not needing import, product cost is per ton compares low 1～2,000 yuan than like product.

5. nontoxic.Liquid 351 of the present invention is directly or indirectly to contact with human body, and employed starting material are nontoxic product; The raw material that can be used as washing powder, washing liquid, washing cream and perfumed soap.

Embodiment

1. the composition of liquid 351 and content (weight percent):

1. 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl (coarse filtration cake) (popular name CF-351), molecular weight: 562.6, content 22%; Its structure is:

English name is: Benzenesulfonic, acid

2，2′-[(1，1-biphenyl)-4，4-diydldi-2，1-ethenediyl]bis-di sodium salt

2. emulsifying agent is the TX-10 (polyoxyethylene nonylphenol ether, English name is: nonylphenyl polyoxyethylene ether, molecular weight 666) in the polyoxyethylene nonylphenol ether (being commonly called as TX series), content 23%;

3. glycerol (popular name glycerine), content 9%;

4. 1,2-propylene glycol, content 18%;

5. deionized water, content 28%.

2. preparation process

With TX-10, glycerine, 1,2--propylene glycol, deionized water add in the there-necked flask successively, adopt water-bath, Electric stove heating system to heat up, when treating that temperature rises to 70 ℃, begin to add CF-351 coarse filtration cake, adopt manual intermittent feeding mode, feed rate is decided according to the dissolution rate of filter cake, add again after filter cake dissolves substantially with added and be advisable for the second time, the coarse filtration cake needs to add in 1.5 hours, controls 70 ℃ of constant temperature again, keeps reaction 3 hours, cold water is cooled to 30 ℃, discharging; Vacuum filtration elimination impurity is collected filtrate and partly is liquid CF-351.

Differential responses condition embodiment experimental result is shown in table 1, table 2 and table 3.

Table 1. differential responses temperature is to the influence of liquid 351

Sample number	1	2	3	4	5	6	7	8	9
										Temperature (℃)	52	55	56	60	65	70	75	80	85
The reinforced time (h)	2.5	2.5	2	2	2	1.5	1.5	1.5	1.5
										Preserve fate	60	60	60	60	60	60	60	60	60

The ingredient groups of respectively organizing sample in the table 1 becomes: 23% TX-10,9% glycerine, 18% 1,2--propylene glycol, 6% deionized water, 44% coarse filtration cake (wherein the amount of effective ingredient CF-351 is 50%, and surplus is a water).

The table 2. differential responses time is to the influence of liquid 351

Sample number	1	2	3	4	5	6	7	8	9
										Reaction times (h)	2	2.5	3	3.5	4	4.5	5	5.5	6
Preserve fate	1	35	44	51	56	60	60	56	55

Respectively organizing the batching of sample in the table 2 forms identical with table 1.

The different CF-351 content of table 3. are to the influence of liquid 351

Sample number	1	2	3	4	5	6	7	8	9	10	11
												CF-351 content (%)	15.5	16	17	18	19	20	21	22	23	24	25
Preserve fate	60	60	60	60	60	60	60	60	30	12	5

The blending process of respectively organizing sample in the table 3 is: get 23 parts TX-10 by weight, 9 parts glycerine, 18 parts 1, the 2--propylene glycol, 6 parts deionized water, the add-on of coarse filtration cake is determined (wherein the amount of effective ingredient CF-351 is 50%, and surplus is a water) by effective ingredient shown in the table 3.

Institute of the present invention synthetic liquid 351 is preserved in the assurance standard under the prerequisite of fate, and adopting the ultraviolet spectrometry scanning method to measure its optical extinction coefficient is 259, surpasses the optical extinction coefficient value of same amount CF-351; Adopt high performance liquid chromatography (area normalization) method, measuring its content is 22%, substantially exceeds the content that can make among the WO 01/127771.

Claims (6)

1. a white dyes is characterized in that, its weight consists of:

4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl is greater than 15% to less than 25%, polyoxyethylene nonylphenol ether 20～30%, glycerol 5～15%, propylene glycol 15～30%, deionized water 5～40%.

2. according to the described white dyes of claim 1, it is characterized in that: described propylene glycol is 1, the 2-propylene glycol.

3. according to the described white dyes of claim 1, it is characterized in that: described 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-the biphenyl weight content is 1 6～22%.

4. according to the described white dyes of claim 1, it is characterized in that: described 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-the biphenyl weight content greater than 20% to less than 25%.

5. according to the described white dyes of claim 1, it is characterized in that:

The weight content of described each component is: 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl 22%, polyoxyethylene nonylphenol ether 23%, glycerol 9%, propylene glycol 18%, deionized water 28%.

6. the preparation method of the described white dyes of claim 1 is characterized in that:

1) with after polyoxyethylene nonylphenol ether, glycerol, propylene glycol, the deionized water mixing, is warming up to 52～80 ℃;

2) adding 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl; Adopt the feed way of intermittent type or continous way, feed rate according to 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-dissolution rate of biphenyl coarse filtration cake and decide, 4,4 '-(2-sulfonic benzo vinyl)-1,1 '-biphenyl coarse filtration cake need add in 1.5 hours;

3) isothermal reaction is 2～6 hours, and cold water is cooled to 30 ℃ with bottom discharge; Filter elimination impurity, collect filtrate and partly be finished product.