Technique for preparing white carbon black by phosphoric acid precipitation and directly coproducing sodium phosphate

A technology of sodium phosphate and white carbon black, applied in the field of sodium phosphate, can solve the problems of discount of application value and economic value, difficult process technology, and reduced product quality, etc., to solve the pressure of environmental protection, improve adaptability, Inclusion reduction effect

Active Publication Date: 2012-09-05
HUBEI XINGFA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese Patent Publication No. CN1686792A discloses a "preparation method of phosphoric acid precipitated silica", and there are two outstanding problems in this method. 2 .nH 2 O or SiO 2 The physical package in the adsorption capacity is very strong, when using H 3 PO 4 When used as an acidifying curing agent, it is difficult to wrap and absorb the crystallized filter cake in SiO after filtration. 2 .nH 2 O or SiO 2 Phosphorus or phosphate compounds in the solids are washed and removed to meet the requirements of use, and the consequence is that the residual phosphorus content in the final product is relatively high
If NaCl phosphate is recovered separately from the mother liquor when water is recovered, the technical difficulty will be very large and troublesome, and the production cost will increase significantly; if the two are recovered as a mixed salt with a mixture, the product The quality is greatly reduced, and the application value and economic value are greatly reduced
Therefore, the auxiliary method of adding NaCl electrolyte to the reaction system for gel precipitation, no matter in terms of technical difficulty or economic cost, will lead to more disadvantages than advantages, and the effect of getting twice the result with half the effort

Method used

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  • Technique for preparing white carbon black by phosphoric acid precipitation and directly coproducing sodium phosphate
  • Technique for preparing white carbon black by phosphoric acid precipitation and directly coproducing sodium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add sodium silicate with a weight of 1000g, a modulus of 3.1, and a content of 34.56% and a phosphoric acid solution with a content of 60% in two 1000ml containers to ensure that the molar ratio of sodium to phosphorus is 1.0. At 80°C, add at a constant speed at the same time, and react for 15 minutes in an 80°C constant temperature reaction vessel with rapid stirring. Add 25 ml of nitric acid with a volume ratio of 1:1, and continue stirring for 3 minutes. Vacuum filter while hot, wash once with water, recover the reaction filtrate and wash filtrate once, then wash with water until the pH is 3.5-5.5, and recover the filtrate for washing of the next batch of materials. Dry at 105°C for 2 hours, grind, add dilute nitric acid and stir thoroughly, filter with suction, wash with water, filter with suction until neutral, and recover the filtrate. The resulting filter cake is dried at 105°C and crushed to become a white carbon black product.

[0029] Sodium silicate modulus...

Embodiment 2

[0031] Add sodium silicate with a weight of 1000g, a modulus of 3.1, and a content of 34.56% and a phosphoric acid solution with a content of 60% in two 1000ml containers respectively to ensure that the molar ratio of sodium to phosphorus is 0.9, and keep the temperature in a water bath to At 90°C, add at a constant speed at the same time, and react for 15 minutes in a 90°C constant temperature reaction vessel with rapid stirring. Add 25 ml of nitric acid with a volume ratio of 1:1, and continue stirring for 3 minutes. Vacuum filter while hot, wash once with water, recover the reaction filtrate and wash filtrate once, then wash with water until the pH is 3.5-5.5, and recover the filtrate for washing of the next batch of materials. Dry at 105°C for 2 hours, grind, add dilute nitric acid and stir thoroughly, filter with suction, wash with water, filter with suction until neutral, and recover the filtrate. The resulting filter cake is dried at 105°C and crushed to become a white...

Embodiment 3

[0033] Add sodium silicate with a weight of 1500g, a modulus of 3.1, and a content of 34.56% and a phosphoric acid solution with a content of 60% in two 1000ml containers to ensure that the molar ratio of sodium to phosphorus is 0.95. At 90°C, add at a constant speed at the same time, and react for 15 minutes in a 90°C constant temperature reaction vessel with rapid stirring. Add 25 ml of nitric acid with a volume ratio of 1:1, and continue stirring for 3 minutes. Vacuum filter while hot, wash once with water, recover the reaction filtrate and wash filtrate once, then wash with water until the pH is 3.5-5.5, and recover the filtrate for washing of the next batch of materials. Dry at 105°C for 2 hours, grind, add dilute nitric acid and stir thoroughly, filter with suction, wash with water, filter with suction until neutral, and recover the filtrate. The resulting filter cake is dried at 105°C and crushed to become a white carbon black product.

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Abstract

The invention relates to a technology for preparing white carbon black by the phosphoric acid precipitation method and directly co-producing sodium phosphate, which comprises homoeothermal co-current flow feeding with the same ratio and heat-insulated reaction, the operating method for controlling gel by violent stirring, and a technological method for liquid solid extraction, purification and washing and removal of residual phosphor. The technology takes sodium silicate and industrial phosphoric acid as raw materials, controls the adding method, the mol ratio of sodium elements to phosphor elements, the reaction temperature, constant-temperature reaction and the operating method for controlling gel particles by violent stirring, adds a given filter aid to improve the filter condition, and adds an extractant to wash away residual phosphor in the white carbon black, so that the product which completely accords with the use requirements is obtained and simultaneously the added filter aid does not influence the use value of by-products and the purity of the obtained by-product monosodium orthophosphate is higher.

Description

technical field [0001] The present invention relates to the process of using phosphoric acid and sodium silicate as raw materials to produce low-residual phosphorus white carbon black product by precipitation method, and co-produce sodium phosphate salt with industrial value, especially a kind of phosphoric acid precipitation method to prepare white carbon black and directly Co-production of sodium phosphate salt process. Background technique [0002] First of all, using sulfuric acid or hydrochloric acid and sodium silicate as raw materials, the technology of preparing white carbon black by precipitation method is complete and has a long history. With the development of the times, the advancement of technology, the improvement of environmental protection requirements, the concept of making full use of resources and optimizing technical and economic indicators continues to deepen. Using sulfuric acid or hydrochloric acid as the raw material to produce sodium sulfate or sodiu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12C01B25/30
Inventor 熊祥祖李少平杨丞杰罗光典王威余有平
Owner HUBEI XINGFA CHEM GRP CO LTD
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