CN101580644A - Pollution-free preparation technology of direct fast yellow D-RL - Google Patents

Abstract

The invention discloses a polyurea formaldehyde coated with organic tin compound microcapsule and a preparation method thereof. The invention adopts an in-situ polymerization method, takes urea and formaldehyde as main wall material raw materials, takes a catalyst organic tin compound as a main capsule core raw material, takes water as a reaction medium, selects surface active agents of different varieties and adjusts the pH value of a reaction solution system to 4 to 5 by controlling a certain rotating speed, the reaction temperature is 30 DEG C to 50 DEG C, and the polyurea formaldehyde coated with organic tin compound microcapsule is obtained by synthesis after the reaction is carried out for 2 to 4 hours; and white microcapsule particles are obtained by carrying out water/acetone washing, leaching and drying on the reaction product. The polyurea formaldehyde coated with organic tin compound microcapsule synthesized by adopting the in-situ polymerization method has simple technology operation and easy control, the yield of synthesized microcapsule products is 85% to 95%, and the polyurea formaldehyde coated with organic tin compound microcapsule can be used for the control of the solidification reaction of thermosetting resin and the toughening and modification of correlative materials simultaneously.

Description

Direct fast yellow D-RL pollution-free preparation process

Technical field

The present invention relates to a kind of preparation technology of dyestuff, particularly a kind of direct fast yellow pollution-free preparation process.

Background technology

At present, the competition of substantive dyestuff industry is growing more intense, and people require also improving constantly to the textiles color, and also more and more higher to the requirement of dyestuff, bright in luster, that dye uptake is high environmental protection dyestuff, salt-free liquid dye are favourably welcome.

In the traditional processing technology of substantive dyestuff, generally through oversalting, filtration with technological process such as concentrate; Purpose is desalination, removes unreacted raw material, intermediate and secondary dyestuff, sloughs moisture, to obtain the dyestuff of desired concn and purity, carries out oven drying then, and making powder dye or directly preparing becomes liquid dye.Facts have proved that the impurity, the salinity that bring in the synthetic and salting-out process have compiled a large amount of compositions that influence dyestuffs purity, intensity and solubleness, have only the impurity that reduces in the dyestuff, tinctorial strength that salinity could improve dyestuff and dyestuffs purity etc.At present, domestic traditional DYE PRODUCTION technology mainly adopts saltouts or acid out separation dyestuff composition, and product purity is not high, and the quality product consistence of different batches is also relatively poor, and quality product is very limited.Moreover owing to used a large amount of sodium-chlor at salting-out process, can produce a large amount of waste water again, the discharging of waste water not only makes useful matteies such as the industrial chemicals that wherein contains and intermediate slattern, and also can cause great pollution to environment, is seriously restricting the Sustainable development of dyestuffs industries.

For example, existing direct fast yellow D-RL is one of kind important in the substantive dyestuff, also is the wider dyestuff of a kind of range of application.Yet, having produced a large amount of waste water in this dyestuff traditional processing technology, not treated discharging can cause serious environmental to pollute.And can improve the cost of product to the processing of processing wastewater.

Therefore, how to simplify production technique, waste water consumption in technology, is improved the dyestuff quality, energy-saving and cost-reducing, minimizing is polluted, and is one of current urgent problem of substantive dyestuff industry.

Summary of the invention

The objective of the invention is to overcome above-mentioned weak point, a kind of direct fast yellow D-RL pollution-free preparation process of simplifying production technique, raising dyestuff quality, reducing production costs, purify production environment is provided.

Implementation step of the present invention for achieving the above object is as follows:

(1) preparation 3-(4-amino-2-tolyl) azo-1, the dissolving of 5-naphthalene disulfonic acid:

In the 300L reactor, add water 200L, add 21.05Kg, 3-(4-amino-2-tolyl) azo-1, making beating is 30 minutes behind the 5-naphthalene disulfonic acid, adds soda ash again and adjusts pH=6～6.5, and this moment, material was a clear solution;

(2) cyanuric chloride making beating:

Add water 50L in volume is the jar of 700L, adds cyanuric chloride 4.7Kg again, adjust temperature t=0～5 ℃ with ice cube, it is standby to start stirring to pulp 45～60 minutes;

(3) primary condensation:

With ready 3-(4-amino-2-tolyl) azo-1,5-naphthalene disulfonic acid solution joined in 1 hour in the cyanuric chloride of having pulled an oar, controlled pH=5～5.5 in the reinforced process, temperature t=0～5 ℃; In 15～20 minutes, add 20% soda ash then and adjust pH=6.1～6.5, kept this Conditioning 4～4.5 hours;

(4) secondary condensation:

In 30～40 minutes, be warming up to t=40～45 ℃ behind the primary condensation terminal point, add 20% soda ash and adjust pH=7.3～7.5, keep acting on 4～5 hours under this condition, checked PH values and temperature in the reaction process in per 20 minutes;

(5) three condensations:

After the secondary condensation finished, disposable quick adding 2.14Kg thanomin was rapidly heated then to t=90～95 ℃; If medium is low in the reaction process, can add soda ash solution and keep pH=9～9.5, to check pH value and temperature in the mechanism, 5～7 hours reaction times;

Material directly send the drying tower spraying drying behind the reaction terminating, sets inlet temperature: 227 ℃; Temperature out: 103 ℃; Be prepared into hollow bead shape solid dye, particle diameter is 1～1.3mm.

The invention has the beneficial effects as follows:

Cleaning of non-wastewater discharge produced and save energy in the outstanding embodiment of this production technique production technique.Change direct fast yellow D--RL traditional processing technology condition, main remove saltout, press filtration, pulping process, adopt the direct spray method of magma.Save former subsidiary material, saved the 10%-20% sodium-chlor that traditional method adds in proportion; It is good that spray-dried tower is handled the back consistency of product, both saved time, economizes coal, power saving, province's steam etc.For example, general substantive dyestuff is produced 300kg/h, and the inventive method is produced 500kg/h-800kg/h.Simplify production technique, reduce production costs, effectively improved quality product, increased product yield, enlarged throughput, and fundamentally solved the contaminated wastewater problem of environment.

Facts have proved that the impurity that brings in the synthetic and salting-out process of dyestuff, purity, intensity and the solubleness that salt branch greatly influences dyestuff have only the salinity that reduces in the dyestuff could improve the tinctorial strength of dyestuff.Water-insoluble can reach 0.05%, be better than traditional technology greatly, can directly produce the consistence that keeps the different batches quality product, eliminate the high density colorful wastewater that produces in the salting-out process, and create a stable solvent condition for adding auxiliary by the spray-drying tower serialization.Save traditional saltout, filter-pressing process has then alleviated waste water from dyestuff from the source intractability, help the smooth implementation of efforts at environmental protection.

Description of drawings

Fig. 1 is a process flow sheet of the present invention;

Among the figure: yellow bass is 3-(4-amino-2-tolyl) azo-1, the 5-naphthalene disulfonic acid.

Embodiment

Below in conjunction with accompanying drawing and preferred embodiment, to details are as follows according to embodiment provided by the invention:

As shown in Figure 1, a kind of direct fast yellow D-RL pollution-free preparation process is characterized in that implementation step is as follows:

(1) the yellow bass dissolving of preparation is 3-(4-amino-2-tolyl) azo-1, the dissolving of 5-naphthalene disulfonic acid:

In the 300L reactor, add water 200L, add 21.05Kg, 3-(4-amino-2-tolyl) azo-1, making beating is 30 minutes behind the 5-naphthalene disulfonic acid, adds soda ash again and adjusts pH=6～6.5, and this moment, material was a clear solution;

(2) cyanuric chloride making beating:

Add water 50L in volume is the jar of 700L, adds cyanuric chloride 4.7Kg again, adjust temperature t=0～5 ℃ with ice cube, it is standby to start stirring to pulp 45～60 minutes;

(3) primary condensation:

With ready 3-(4-amino-2-tolyl) azo-1,5-naphthalene disulfonic acid solution joined in 1 hour in the cyanuric chloride of having pulled an oar, controlled pH=5～5.5 in the reinforced process, temperature t=0～5 ℃; In 15～20 minutes, add 20% soda ash then and adjust pH=6.1～6.5, kept this Conditioning 4～4.5 hours;

(4) secondary condensation:

In 30～40 minutes, be warming up to t=40～45 ℃ behind the primary condensation terminal point, add 20% soda ash and adjust pH=7.3～7.5, keep acting on 4～5 hours under this condition, checked PH values and temperature in the reaction process in per 20 minutes;

(5) three condensations:

After the secondary condensation finished, disposable quick adding 2.14Kg thanomin was rapidly heated then to t=90～95 ℃; If medium is low in the reaction process, can add soda ash solution and keep pH=9～9.5, to check pH value and temperature in the mechanism, 5～7 hours reaction times;

Material directly send the drying tower spraying drying behind the reaction terminating, sets inlet temperature: 227 ℃; Temperature out: 103 ℃; Be prepared into hollow bead shape solid dye, particle diameter is 1～1.3mm.

The chemical structural formula of described direct fast yellow D-RL:

Table 1: the technical indicator contrast of the inventive method and produced in conventional processes product is as follows:

The key technical indexes	The inventive method	Traditional method
			Water-insoluble	0.05％	0.2％
Solubleness	80g/L	70g/L
			The pH value	7.5	7.5
Light fastness	4～5 grades	3～4 grades

The index that dye solution solid content that the inventive method is produced and intensity significantly are better than adopting prior art; Effectively improve the yield and the tinctorial strength of dyestuff, have very strong competitive power with its stable quality, preferential price, make product improve a class, market outlook are boundless.Simultaneously, the present invention reduces the generation of pollutent in the production process to greatest extent, carries out cleaner production.Can reduce waste discharge significantly, the pollution problem that fundamentally solves dye industry.DYE PRODUCTION economic benefit of the present invention is very remarkable, and its development prospect is very optimistic, has enormous potentialities.

Above-mentioned with reference to embodiment to the detailed description that this direct fast yellow D-RL pollution-free preparation process carries out, be illustrative rather than determinate, therefore, should belong within protection scope of the present invention in the variation and the modification that do not break away under the general plotting of the present invention.

Claims (1)

1, a kind of direct fast yellow D-RL pollution-free preparation process is characterized in that implementation step is as follows:

(1) preparation 3-(4-amino-2-tolyl) azo-1, the dissolving of 5-naphthalene disulfonic acid:

In the 300L reactor, add water 200L, add 21.05Kg, 3-(4-amino-2-tolyl) azo-1, making beating is 30 minutes behind the 5-naphthalene disulfonic acid, adds soda ash again and adjusts pH=6～6.5, and this moment, material was a clear solution;

(2) cyanuric chloride making beating:

Add water 50L in volume is the jar of 700L, adds cyanuric chloride 4.7Kg again, adjust temperature t=0～5 ℃ with ice cube, it is standby to start stirring to pulp 45～60 minutes;

(3) primary condensation:

With ready 3-(4-amino-2-tolyl) azo-1,5-naphthalene disulfonic acid solution joined in 1 hour in the cyanuric chloride of having pulled an oar, controlled pH=5～5.5 in the reinforced process, temperature t=0～5 ℃; In 15～20 minutes, add 20% soda ash then and adjust pH=6.1～6.5, kept this Conditioning 4～4.5 hours;

(4) secondary condensation:

In 30～40 minutes, be warming up to t=40～45 ℃ behind the primary condensation terminal point, add 20% soda ash and adjust pH=7.3～7.5, keep acting on 4～5 hours under this condition, checked PH values and temperature in the reaction process in per 20 minutes;

(5) three condensations:

After the secondary condensation finished, disposable quick adding 2.14Kg thanomin was rapidly heated then to t=90～95 ℃; If medium is low in the reaction process, can add soda ash solution and keep pH=9～9.5, to check pH value and temperature in the mechanism, 5～7 hours reaction times;

Material directly send the drying tower spraying drying behind the reaction terminating, sets inlet temperature: 227 ℃; Temperature out: 103 ℃; Be prepared into hollow bead shape solid dye, particle diameter is 1～1.3mm.

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