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Preparation method of 2,7-sodium naphthalenedisulfonate product using transforming production of 1,6-naphthalenedisulfonic mother liquid

A technology of mother naphthalene disulfonate and sodium naphthalene disulfonate, which is applied in the preparation of sulfonate salts and organic chemistry, and can solve the problems of difficult treatment, unfavorable environmental protection, and large amount of mother liquor, so as to improve economic benefits and reduce the discharge of three wastes , The effect of low production cost

Active Publication Date: 2013-09-18
ZAOZHUANG TAIRUI FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Fourth, it can be seen from its technological process that the mother liquor to the sewage treatment plant contains a large amount of sodium sulfate, sodium chloride, sodium 2,7-naphthalene disulfonate, sodium 2,6-naphthalene disulfonate and sulfuric acid hydrochloric acid, etc. Other impurities, and the amount of mother liquor is large, difficult to handle, high cost, not only unfavorable to environmental protection, but also causes great economic pressure on enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of new method that utilizes 1,6-naphthalene disulfonic acid product mother liquor conversion to produce 2,7-naphthalene disulfonic acid sodium product, comprises the steps:

[0026] 1. Pump 2600kg of 1,6-naphthalene disulfonic acid mother liquor into the reactor, distill water under reduced pressure, and the vacuum degree is -0.08Mpa.

[0027] 2. When the temperature rises to 170°C, the detected moisture is 14.3%, stop distilling water.

[0028] 3. Add 440kg of naphthalene and 770kg of sulfuric acid, and heat it to 180°C for 5 hours.

[0029] 4. Transfer the reaction solution to a transfer kettle, cool it down to 110°C and pump it into a hydrolysis kettle filled with 1000kg of water, and the hydrolysis temperature must not exceed 130°C.

[0030] 5. The hydrolyzed solution was stirred for half an hour and then cooled to 10° C. and centrifuged to obtain 2,7-naphthalene disulfonic acid with a yield of 800 kg and a purity of 93%.

[0031] 6. Salt formation to obtai...

example example 2

[0033] A kind of new method that utilizes 1,6-naphthalene disulfonic acid product mother liquor conversion to produce 2,7-naphthalene disulfonic acid sodium product, comprises the steps:

[0034] 1. Pump 2600kg of 1,6-naphthalene disulfonic acid mother liquor into the reactor, distill water under reduced pressure, and the vacuum degree is -0.095Mpa.

[0035] 2. When the temperature rises to 180°C, the detected moisture is 14.8%, stop distilling water.

[0036] 3. Add 440kg of naphthalene and 770kg of sulfuric acid, heat it to 183°C and keep it warm for 5 hours.

[0037] 4. Transfer the reaction solution to a transfer kettle, cool it down to 110°C and pump it into a hydrolysis kettle filled with 1000kg of water, and the hydrolysis temperature must not exceed 130°C.

[0038] 5. The hydrolyzed solution was stirred for half an hour, then cooled to 15°C and centrifuged to obtain 2,7-naphthalene disulfonic acid with a yield of 830 kg and a purity of 93.1%.

[0039] 6. Salt formati...

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PUM

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Abstract

The invention discloses a preparation method of a 2,7-sodium naphthalenedisulfonate product using transforming production of 1,6-naphthalenedisulfonic mother liquid. The method is characterized by comprising the following steps of: (I) pumping 1,6-naphthalenedisulfonic mother liquid containing 30-70% of water into a reaction kettle, and performing reduced-pressure concentration, wherein the vacuum degree is -0.08 to -0.095 Mpa, and the temperature does not exceed 180 DEG C; (II) when the water content is 14-15%, stopping heating; (III) adding naphthalene and sulfuric acid, heating to 180-190 DEG C, and preserving heat for 5 hours; (IV) after cooling to 110-120 DEG C, and transferring the reaction liquid into a transfer kettle, and after cooling down to 120 DEG C, pumping the reaction liquid into a hydrolysis kettle with water, wherein the hydrolysis temperature does not exceed 130 DEG C; (V) stirring for half an hour, cooling to 10-20 DEG C, and centrifuging to obtain 2,7-naphthalene disulfonic acid; and (VI) salifying to obtain 2,7-sodium naphthalenedisulfonate. The method disclosed by the invention has low cost, requires small investment and discharges little three wastes (waste gas, waste water and individual residue).

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method for producing sodium 2,7-naphthalene disulfonate product by converting the mother liquid of 1,6-naphthalene disulfonic acid product. Background technique [0002] Produce 2 at present, the technique of 7-sodium naphthalene disulfonate is as follows: [0003] 1. Concentrating the mother liquor of 1,6-naphthalene disulfonic acid under reduced pressure; [0004] 2. Add sulfuric acid, refined naphthalene and catalyst to the concentrated solution; [0005] 3. Lower the temperature of the reaction solution to below 100°C, add sodium chloride and sodium sulfate to stir, maintain the negative pressure of the system, and remove the hydrogen chloride; [0006] 4. Filtrating the liquid-solid mixture with heat preservation to obtain thick sodium 2,6-naphthalene disulfonate solid and filtrate I; [0007] 5. Wash the obtained thick sodium 2,6-naphthalene dis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/35C07C303/32
Inventor 杨玉栋周志辉
Owner ZAOZHUANG TAIRUI FINE CHEM