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A method for preparing basic chromium sulfate by utilizing the raffinate obtained from the production of menadione

A technology for obtaining menadione and chromium sulfate, applied in directions such as chromium sulfate, can solve problems such as slow curing reaction rate, environmental pollution, waste of resources, etc., and achieve the effects of improving production efficiency, shortening curing time, and accelerating curing reaction

Active Publication Date: 2016-05-18
SICHUAN YINHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of naphthoquinone raffinate produced at the same time contains a large amount of hexavalent chromium and strong acid. If not utilized, it will not only cause a great waste of resources, but also may cause serious environmental pollution.
In addition, menadione raffinate contains methylnaphthalene and its derivatives, if it cannot be effectively removed, it will seriously affect the quality of basic chromium sulfate
[0005] At present, the production of basic chromium sulfate products is almost all prepared by menadione raffinate, which makes the problem of excessive organic content in basic chromium sulfate exist for a long time
In addition, due to the preparation of basic chromium sulfate by the reduction method, the aging reaction rate is relatively slow, generally more than 8 hours, which seriously affects the production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Step 1, with 2000mL, 60g / L menadione raffinate (with Na 2 Cr 2 o 7 meter) was evaporated and concentrated to 42 Baume degrees, and the residue was removed by filtration;

[0049] Step 2, in the pressure reactor, 910mL concentrated filtrate (with Na 2 Cr 2 o 7 Calculated) by adding 82.4g glucose (in C 6 h 12 o 6 Meter) mixed, at 150 ℃, 1.2MPa, react for 1h;

[0050] After the reaction of step 3 and step 2 is finished, take a sample to detect the content of hexavalent chromium, and then add sodium pyrosulfite, sodium pyrosulfite and Na 2 Cr 2 o 7 The mol ratio is 1.5:1, and stirring reaction 2h under normal temperature, normal pressure, the unreduced hexavalent chromium in feed liquid is all converted into trivalent chromium;

[0051] Step 4: Add sodium hydroxide solution to the feed solution obtained in Step 3, adjust the basicity to 33.05%, then filter, and dry the filtered slurry at 80° C. for 2 hours to obtain 76 g of basic chromium sulfate product.

[005...

Embodiment 2

[0056] Step 1, 2000mL, 85g / L menadione raffinate (calculated as Na2Cr2O7) is evaporated and concentrated to 45 degrees Baume, and the slag is removed by filtration;

[0057] Step 2, in the pressure reactor, the 890mL concentrated filtrate (in the form of Na 2 Cr 2 o 7 Calculated) Add 116.8g of starch (in C 6 h 12 o 6 (meter) mixed, and reacted for 1.5h at 200°C and 1.8MPa;

[0058] Step 3, step 2 After the reaction is over, take a sample to detect the content of hexavalent chromium, and then add sodium bisulfite, sodium bisulfite and Na 2 Cr 2 o 7 The mol ratio is 3:1, and stirring reaction 3h under normal temperature, normal pressure, the unreduced hexavalent chromium in feed liquid is all converted into trivalent chromium;

[0059] Step 4: Add sodium hydroxide solution to the feed solution obtained in step 3, adjust the basicity to 33.42%, then filter, and dry the filtered slurry at 80° C. for 2 hours to obtain 107 g of basic chromium sulfate product.

[0060] The t...

Embodiment 3

[0064] Step 1, with 2000mL, 108g / L menadione raffinate (with Na 2 Cr 2 o 7 meter) evaporated and concentrated to 50 Baume degrees, filtered to remove residue;

[0065] Step 2, in pressure reactor, with 900mL concentrated filtrate (with Na 2 Cr 2 o 7 Calculated) by adding 148.4g glucose (in C 6 h 12 o 6 Meter) mixed, at 250 ℃, 2.6MPa, reaction 2h;

[0066] After the reaction of step 3 and step 2 is completed, take a sample to detect the content of hexavalent chromium, and then add sodium sulfite, sodium sulfite and Na 2 Cr 2 o 7 The mol ratio is 3:1, and stirring reaction 4h under normal temperature, normal pressure, the unreduced hexavalent chromium in feed liquid is all converted into trivalent chromium;

[0067] Step 4: Add sodium hydroxide solution to the feed solution obtained in step 3, adjust the basicity to 33.67%, then filter, and dry the filtered slurry at 80° C. for 2 hours to obtain 136 g of basic chromium sulfate product.

[0068] The test results of th...

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Abstract

The invention discloses a method for preparing chromium sulfate basic by utilizing residual liquor obtained during menadione production. The method comprises the following steps: uniformly mixing the concentrated residual liquor with industrial sugar according to a certain molar ratio, and reacting in a pressure reactor for 0.5-4 hours at the temperature of 100 to 300 DEG C under the pressure of 0 to 4MPa; completely reducing a small amount of unreacted hexavalent chromium in the feed liquid into trivalent chromium by using a reducing agent after the reaction is ended; regulating the basicity of the feed liquid by using an alkaline solution, filtering, performing spray drying on the filtrate, thus obtaining the chromium sulfate basic product. According to the method disclosed by the invention, a pressure-conditioned curing reaction is adopted, residual organic matters in the menadione residual liquor can be effectively removed, and the quality of chromium powder is improved. The method disclosed by the invention is simple in process, high in reaction rate, low in energy consumption, clean and environment-friendly.

Description

technical field [0001] The invention relates to a method for preparing basic chromium sulfate by utilizing the raffinate obtained from the production of menadione, in particular to a method for producing basic chromium sulfate by using industrial sugar to reduce menadione raffinate containing sodium rubidone in a pressure reaction kettle. Background technique [0002] Both chromium sulfate and basic chromium sulfate can be used to make chromium hydroxide and other chromium salts. Chromium sulfate is used for printing and dyeing, ceramics, metal passivation and trivalent chromium electroplating, and basic chromium sulfate is mainly used for tanning leather. It can be miscible with zirconium sulfate, aluminum sulfate, etc. to make chrome aluminum tanning agent or chrome aluminum zirconium tanning agent, mix with masking agent to make masking type tanning agent, and crosslink with dibasic acid to make crosslinked tanning agent. [0003] The production process of basic chromium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G37/08
CPCC01G37/08
Inventor 李先荣陈宁董明甫黄玉西谢友才袁小超李逢彬
Owner SICHUAN YINHE CHEM
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