Unlock instant, AI-driven research and patent intelligence for your innovation.

A method of co-producing citric acid and calcium sulfate dihydrate

A technology of calcium sulfate dihydrate and calcium sulfate hemihydrate, which is applied in the fields of calcium/strontium/barium sulfate, carboxylate preparation, organic chemistry, etc. Loss and other problems, to achieve the effect of reducing equipment and environment requirements, easy solid-liquid separation and washing, and reducing safety hazards

Inactive Publication Date: 2011-11-30
COFCO BIOTECHNOLOGY CO LTD
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its disadvantages are also obvious. Due to the need to react at a higher temperature, the easy carbides entrained in calcium citrate will be carbonized by concentrated sulfuric acid, and the chroma of the citric acid solution obtained by the reaction will increase; The solubility of calcium sulfate dihydrate in citric acid aqueous solution is higher than the solubility of calcium sulfate dihydrate in citric acid aqueous solution. After solid-liquid separation, the content of calcium ions and sulfate ion in citric acid aqueous solution is high, which will pollute the resin and increase the regeneration frequency; the temperature of the reaction solution is high, Improve the equipment and environment requirements for subsequent solid-liquid separation. At the same time, there are potential safety hazards caused by high temperature during solid-liquid separation, and relevant safety precautions are required.
[0006] The reactant calcium citrate is solid, and the product calcium sulfate is also solid. When the sulfuric acid is added too fast, too slowly, stopped midway or stirred unevenly during the reaction, calcium sulfate will embed calcium citrate. In severe cases, there will be agglomeration (caking) of materials in the reaction tank
The entrapment of calcium citrate salt reduces the purity of calcium sulfate and causes the loss of citric acid yield, which makes subsequent solid-liquid separation difficult. This phenomenon cannot be completely avoided by the above two production processes.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method of co-producing citric acid and calcium sulfate dihydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Calcium citrate crude product (purity 94.1% by weight, moisture content 36.9% by weight) is slurried with water, the content of water in the obtained calcium citrate slurry is 50% by weight, and the concentrated sulfuric acid of calcium citrate slurry and 98% by weight is mixed with 4m 3 The feed rate of / h is continuously added to the first-stage reaction tank, the temperature of the reaction liquid in the first-stage reaction tank is controlled at 93°C, and the conductivity of the reaction liquid is controlled to be 12±3mS / cm. When the liquid level of the reaction tank reaches 4m 3 When , the material in the first-stage reaction tank is input to the second-stage reaction tank, and the feeding speed of the material is 4m 3 / h, while maintaining the liquid level of the first-stage reaction tank at 4m 3 .

[0050]Control the temperature of the reaction liquid in the second-stage reaction tank to 85°C, and the conductivity is 4±2mS / cm. When the liquid level of the second...

Embodiment 2

[0054] The thick product (98.2% by weight of purity, 42.2% by weight of moisture) of 1000 parts by weight of calcium hydrogen citrate is slurried with dilute citric acid solution (6.7% by weight of concentration), and the content of water in the calcium hydrogen citrate slurry that obtains is 55% by weight The calcium hydrogen citrate slurry and 98% by weight of concentrated sulfuric acid are added into the reaction tank together, the temperature of the reaction tank is 96°C, the conductivity of the reaction solution is controlled to be 8±2mS / cm, and the reaction time is 50 minutes.

[0055] Under the condition of stirring, the temperature of the reaction tank was lowered to 81°C at an average cooling rate of 0.5°C / min and kept stirring for 50 minutes, and fine-tuned with sulfuric acid or calcium hydrogen citrate slurry to control the conductivity of the reaction solution to 5±1mS / cm.

[0056] Under the condition of stirring, the temperature of the reaction tank was lowered t...

Embodiment 3

[0059] Calcium hydrogen citrate crude product (98.4% by weight of purity, 38.6% by weight of moisture content) is slurried with water, and the content of water in the calcium hydrogen citrate slurry obtained is 45% by weight, and the concentrated sulfuric acid of calcium hydrogen citrate slurry and 98% by weight at 5m 3 The feed rate of / h is continuously added to the first-stage reaction tank, the temperature of the reaction liquid in the first-stage reaction tank is controlled at 94°C, and the conductivity of the reaction liquid is controlled to be 7±1mS / cm. When the liquid level of the reaction tank reaches 4m 3 When , the material in the first-stage reaction tank is input to the second-stage reaction tank, and the material feeding speed is 5m 3 / h, the average cooling rate is 76°C / min, while maintaining the liquid level of the first stage reaction tank at 4m 3 .

[0060] Control the temperature of the reaction liquid in the second-stage reaction tank to 84°C, and the con...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for the co-production of citric acid and calcium sulfate dihydrate. The method comprises the following steps: (1) carrying out contact reaction on calcium citrate and sulfuric acid aqueous solution to obtain a mixed liquid of citric acid and calcium sulfate hemihydrate, wherein the temperature of the contact reaction between the calcium citrate and the sulfuric acid aqueous solution is higher than the transition temperature at which calcium sulfate hemihydrate is converted into calcium sulfate dihydrate; (2) cooling the mixed liquid of citric acid and calcium sulfate hemihydrate to a temperature lower than the transition temperature at which calcium sulfate hemihydrate is converted into calcium sulfate dihydrate, so that calcium sulfate hemihydrate is converted into calcium sulfate dihydrate, thus obtaining a mixed liquid of citric acid and calcium sulfate dihydrate; and (3) carrying out solid-liquid separation on the mixed liquid of citric acid and calcium sulfate dihydrate to obtain citric acid solution and solid-phase calcium sulfate dihydrate. Through the method disclosed by the invention, the content of free water is low in the produced calcium sulfate dihydrate while ensuring low citric acid residues, and the produced citric acid has high concentration (up to 0.6 g / ml or above). The method disclosed by the invention can be widely used in industrial production.

Description

technical field [0001] The invention relates to a method for co-producing citric acid and calcium sulfate dihydrate. Background technique [0002] Calcium sulfate has a wide range of uses, but the calcium sulfate produced by the reaction of calcium citrate and sulfuric acid contains residual citric acid and more free water, which restricts the application of the product calcium sulfate and cannot exert its due value. [0003] The acid hydrolysis of calcium citrate and sulfuric acid produces citric acid and calcium sulfate. There are two traditional methods and ideas. One is to obtain citric acid and calcium sulfate hemihydrate, and the other is to obtain citric acid and calcium sulfate dihydrate. There are three crystal forms of calcium sulfate, which are anhydrous calcium sulfate, hemihydrate calcium sulfate, and dihydrate calcium sulfate. Which crystal form of calcium sulfate is obtained depends on factors such as reaction temperature, reaction time, and reactant concentra...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C59/265C07C51/02C01F11/46
Inventor 张军华王勇顾宗池熊结青王浩
Owner COFCO BIOTECHNOLOGY CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More