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Production method of sodium formaldehyde sulfoxylate powder with low contents of free formaldehyde and zinc

A technology of sodium sulfoxylate and low free formaldehyde, applied in chemical instruments and methods, zinc oxide/zinc hydroxide, sulfur compounds, etc., can solve the problems of high production cost, limitation, complicated operation, etc., and achieve low production cost, Easy-to-control effects

Pending Publication Date: 2018-03-13
江苏勃仑化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The three-step method uses zinc powder, sulfur dioxide and formaldehyde as raw materials to obtain sodium bisulfite formaldehyde through a three-step reaction. This method has a long process flow, a lot of equipment input, complicated operation, high production cost, and serious environmental pollution. Scale promotion and application are limited
But above-mentioned patent is mainly aimed at the diaobai block that three-step method produces, also does not have the method for relevant one-step method production low free formaldehyde low zinc sodium bisulfoxylate formaldehyde (diabai block)
[0006] Diaobaite powder synthesized by one-step method contains a certain amount of zinc ions (100-300ppm) and free formaldehyde (800-1000ppm), which restricts its use in some special application fields (such as medical treatment and rubber industry).

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At 4-6°C, add 100 kg of deionized water, 50 kg of sodium metabisulfite (Na 2 S 2 o 5 ), start stirring, the speed is controlled at 120r / min, and sodium metabisulfite is completely dissolved in deionized water.

[0030] In the above-mentioned stainless steel reaction kettle, add 45 kg of zinc powder (mass fraction 95%, particle size 40 μm). Add 1.5 kg of oxalic acid as an activator to peel off the oxide film on the surface of the zinc powder to restore the activity of the zinc powder. At the same time, the pH of the reaction mixture is controlled to 3.4, the activation temperature is 45°C, and the temperature is kept for 40 minutes.

[0031] In the above-mentioned stainless steel reaction kettle, add 40 kg of formaldehyde solution with a mass fraction of 37%, the temperature is controlled at 48°C, and the temperature is kept for 30 minutes.

[0032] In the above-mentioned stainless steel reaction kettle, feed steam to heat the reaction kettle, raise the temperature to 6...

Embodiment 2

[0038] At 4-6°C, add 100 kg of deionized water, 52 kg of sodium metabisulfite (Na 2 S 2 o 5 ), start stirring, the speed is controlled at 130r / min, and sodium metabisulfite is completely dissolved in deionized water.

[0039] In the above-mentioned stainless steel reaction kettle, add 46 kg of zinc powder (mass fraction 95%, particle size 40 μm). Add 1.6 kg of oxalic acid as an activator to peel off the oxide film on the surface of the zinc powder and restore the activity of the zinc powder. At the same time, the pH of the reaction mixture is controlled to be 3.3, the activation temperature is 42°C, and the temperature is kept for 45 minutes.

[0040] In the above-mentioned stainless steel reaction kettle, add 41 kg of formaldehyde solution with a mass fraction of 37%, control the temperature at 50° C., and keep the temperature for 35 minutes.

[0041] In the above-mentioned stainless steel reaction kettle, feed steam to heat the reaction kettle, raise the temperature to 65...

Embodiment 3

[0047] At 4°C, add 100 kg of deionized water, 48 kg of sodium metabisulfite (Na 2 S 2 o 5 ), start stirring, the speed is controlled at 120r / min, and sodium metabisulfite is completely dissolved in deionized water.

[0048] In the above-mentioned stainless steel reaction kettle, 44 kg of zinc powder (mass fraction 95%, particle size 40 μm) was added. Add 2.0 kg of citric acid as an activator to peel off the oxide film on the surface of the zinc powder and restore the activity of the zinc powder. At the same time, the pH of the reaction mixture is controlled to be 3.5, the activation temperature is 45°C, and the temperature is kept for 40 minutes.

[0049] In the above-mentioned stainless steel reaction kettle, add 39 kg of formaldehyde solution with a mass fraction of 37%, control the temperature at 48° C., and keep the temperature for 30 minutes.

[0050] In the above-mentioned stainless steel reaction kettle, feed steam to heat the reaction kettle, raise the temperature t...

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PUM

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Abstract

The invention relates to a preparation method of a sodium formaldehyde sulfoxylate powder with low contents of free formaldehyde and zinc. Sodium pyrosulfite, zinc powder, and a formaldehyde solutionare taken as the raw materials, an inorganic acid is taken as the activator, and sodium formaldehyde sulfoxylate is produced in one step. After the concentration of sodium formaldehyde sulfoxylate isgreater than 400 g / L, the reactions stop; the temperature is reduced to 40 to 46 DEG C; the reaction system is allowed to stand still to carry out layering; the reaction product is filtered by a plate-and-frame filter press; an inorganic alkali is added into the filtrate to carry out settlement for 40 to 48 hours; zinc in the mother liquor after inorganic alkali settlement is removed, free formaldehyde is removed, and finally evaporation and concentration are performed to obtain blocks of sodium formaldehyde sulfoxylate. The blocks of sodium formaldehyde sulfoxylate are grinded, and filter residues are burned at a high temperature to produce high quality zinc oxide. The stability of prepared sodium formaldehyde sulfoxylate is good, the effective content of sodium formaldehyde sulfoxylate is 97.0 to 99.2%, the zinc content of sodium formaldehyde sulfoxylate is 10 to 30 ppm, and the free formaldehyde content of sodium formaldehyde sulfoxylate is 100-200 ppm. The prepared sodium formaldehyde sulfoxylate can meet special requirements of medicine industry and rubber industry. Na2S2O5+2Zn+2HCHO+2H2O->aHSO2.CHO.H2O+2ZnO.

Description

technical field [0001] The invention relates to a production method of low-free formaldehyde and low-zinc sodium bisulfoxylate formaldehyde (Diaobai block), which belongs to the technical field of chemical industry. Background technique [0002] Sodium bisulfoxylate formaldehyde, also known as sodium formaldehyde sulfoxylate (NaHSO 2 HCHO 2H 2 O), the trade name is Diabaikuai, which has strong reducibility. It is a white blocky substance with strong hygroscopicity. It is easily soluble in water and slightly soluble in alcohol. It is the second generation product of hydrosulfite. Diaobai block is widely used. In the synthetic rubber industry, it can be used as an activator of low-temperature emulsion styrene-butadiene; in the printing and dyeing industry, it can be used as a color-pulling agent; in the pharmaceutical industry, it can be used as an antidote for mercury, bismuth, and barium; Industrial as a reducing agent. At present, there are mainly one-step and three-ste...

Claims

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Application Information

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IPC IPC(8): C07C45/86C07C47/058C01B17/98C01G9/03
CPCC01B17/98C01G9/03C07C45/86C07C47/04
Inventor 宦益宏王国伟周冬梅
Owner 江苏勃仑化学有限公司
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