CN100999327A - Method of extracting industrial anhydrous sodium sulfate from waste water in silicone dioxide production using precipitation method - Google Patents

Method of extracting industrial anhydrous sodium sulfate from waste water in silicone dioxide production using precipitation method Download PDF

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Publication number
CN100999327A
CN100999327A CN 200610102347 CN200610102347A CN100999327A CN 100999327 A CN100999327 A CN 100999327A CN 200610102347 CN200610102347 CN 200610102347 CN 200610102347 A CN200610102347 A CN 200610102347A CN 100999327 A CN100999327 A CN 100999327A
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sodium sulfate
effect evaporator
evaporator
anhydrous sodium
waste water
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CN100513312C (en
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张云升
张乃蛇
邬敦伟
田瑞锋
宋小燕
全慧锋
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Abstract

This invention relates to a preparation method of natrii sulfas exsiccatus. It can extract industrial natrii sulfas exsiccatus from production waste water of precipitating silica, solve problems of low purity of natrii sulfas exsiccatus and high cost about existing preparation method, and filter production waste water of precipitating silica; import waste liquid in evaporator, import steam, concentrate waste liquid; when natrium sulfuricum density achieves 30-35%, centrifugalize and separate; dry natrium sulfuricum, get natrii sulfas exsiccatus. This invention uses filtering- evaporating-drying method to extract industrial natrii sulfas exsiccatus from production waste water of precipitating silica. It can effectively utilize waste water of precipitating silica, avoid environmental pollution of direct releasing, and save energy sources; it gets natrii sulfas exsiccatus of low cost, high purity, low water content, and low calcium, magnesium, and ferri content. It can satisfy requirement of high-quailty natrium sulfuricum.

Description

From the precipitated silica factory effluent, extract the method for industrial anhydrous sodium sulfate
Technical field
The present invention relates to a kind of preparation method of anhydrous sodium sulphate, be specially the method for from the precipitated silica factory effluent, extracting industrial anhydrous sodium sulfate.
Background technology
Anhydrous sodium sulphate belongs to inorganic chemical product, be mainly used in the manufacturing of Chemicals such as sodium sulphite, water glass, in paper industry, be used for sulfate pulping, in glass industry, be used to replace soda ash, in the fuel industry, be used as weighting agent, also be widely used in the industries such as these external printing and dyeing, medicine, washing composition, plating, so at chemical field, its consumption is very big.In the prior art, the preparation of industrial anhydrous sodium sulfate is generally adopted and take nitre mud from natural salt lake, dissolve then nitre liquid, more after filtration, operation such as evaporation, drying produces.The industrial anhydrous sodium sulfate of Sheng Chaning according to the method described above, owing to contain impurity such as a large amount of calcium magnesium, iron, chlorine in the natural nitre mud, be difficult to remove by simple filtration, make that the industrial sulphuric acid sodium product purity that makes is low, cost is high, it is also very narrow to produce approach, has restricted the development of related industries to a certain extent.
Along with the continuous expansion of China's industrial anhydrous sodium sulfate purposes, develop a kind of brand-new, the anhydrous sodium sulphate preparation method has become the hot fields of technological development cheaply.At present, utilizing precipitated silica is that water glass and sulfuric acid prepare the sodium sulfate that comprises 5-7% in the factory effluent of silicon-dioxide (being commonly called as white carbon black), the water more than or equal to 94% and smaller or equal to 1 ‰ silicon-dioxide, but people are used as it as discharge of wastewater now, not only polluted environment, do not meet requirement, and wasted the energy discharge of wastewater.
Summary of the invention
The present invention is problems such as the anhydrous sodium sulphate purity of utilizing prior preparation method to make is low, cost height in order to solve, and a kind of method of extracting industrial anhydrous sodium sulfate from the precipitated silica factory effluent is provided.
The present invention adopts following technical scheme to realize: extract the method for industrial anhydrous sodium sulfate from the precipitated silica factory effluent, may further comprise the steps:
(1) the precipitated silica factory effluent is filtered, reclaim remaining silicon-dioxide and purifying waste;
(2) the above-mentioned waste liquid that obtains is imported vaporizer, and the liquid level in the control vaporizer in evaporator room on liquid level, the steam that feeds temperature then and be 145-160 ℃ is with concentrating spent liquor;
(3) when the concentration of sodium sulfate in the waste liquid reaches 30-35%, it is delivered to whizzer with sodium sulfate and water centrifugation;
(4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 140-150 ℃, and pressure is 0.4-0.55Mpa, promptly gets anhydrous sodium sulphate.
The anhydrous sodium sulphate purity that obtains is higher, foreign matter content is lower in order to make, vaporizer of the present invention is the IV single-effect evaporator, pour the base fluid in the I single-effect evaporator into base fluid that the base fluid in II single-effect evaporator, the II single-effect evaporator pours in III single-effect evaporator, the III single-effect evaporator and pour the IV single-effect evaporator into, the liquid level that guarantees each single-effect evaporator in the said process in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.4-0.5Mpa, and the pressure in the last evaporator is 0.04-0.07Mpa.The present invention adopts the multistage evaporation mode can improve the purity of industrial anhydrous sodium sulfate.
The filter plant that the present invention is adopted in processing step 1 is German import 1.6Mpa autoclave diaphragm filter plant, and at least can be from the Shanxi rich happiness chemical industry equipment of IV single-effect evaporator company limited buys.
Characteristics such as the anhydrous sodium sulphate that adopts preparation technology of the present invention to obtain has that purity height, water content are low, calcium magnesium, iron level are low, check through Shanxi China Coal and Coal Chemical Industry Product Quality Supervision and Ins, every technical indicator all meets or is better than national standard, satisfy the requirement of high quality top grade sodium sulfate fully, see following form:
Project Assay of the present invention National standard
Sodium sulfate Na 2SO 4(%) 99.3 ≥99.00
Calcium magnesium Mg (%) Do not detect ≤0.15
Muriate Cl (%) 0.18 ≤0.35
Iron Fe (%) Do not detect ≤0.002
Moisture content H 2O(%) 0.04 ≤0.10
Whiteness whiteness 85 ≥82
Compared with prior art, the present invention adopts filtration-evaporation-drying means to extract industrial anhydrous sodium sulfate from the precipitated silica factory effluent, preferred and control by processing parameter obtains industrial anhydrous sodium sulfate, effectively utilized the factory effluent of precipitated silica on the one hand, the energy has been saved in the environmental pollution of having avoided direct discharging and having caused; The anhydrous sodium sulphate cost that is obtained on the other hand is low, and purity height, water content are low, calcium magnesium, iron level are low, satisfy the requirement of high quality top grade sodium sulfate fully.
Embodiment
Embodiment 1:
From the precipitated silica factory effluent, extract the method for industrial anhydrous sodium sulfate, may further comprise the steps: (1) filters the precipitated silica factory effluent, reclaim remaining silicon-dioxide and purifying waste adopts German import 1.6Mpa autoclave diaphragm filter plant to filter; (2) the above-mentioned waste liquid that obtains is imported the I single-effect evaporator, pour the base fluid in the I single-effect evaporator into base fluid that the base fluid in II single-effect evaporator, the II single-effect evaporator pours in III single-effect evaporator, the III single-effect evaporator and pour the IV single-effect evaporator into, guarantee in the said process liquid level in each single-effect evaporator in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.4Mpa, pressure in the last evaporator is 0.04Mpa, and the steam that feeds temperature then and be 145 ℃ is with concentrating spent liquor; (3) when the concentration of sodium sulfate in the waste liquid reaches 30%, it is delivered to whizzer with sodium sulfate and water centrifugation; (4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 140 ℃, and pressure is 0.4Mpa, promptly gets the powdery industrial anhydrous sodium sulfate, and the hot steam of each single-effect evaporator generation obtains deionized water after condensation simultaneously.
Embodiment 2:
From the precipitated silica factory effluent, extract the method for industrial anhydrous sodium sulfate, may further comprise the steps: (1) filters the precipitated silica factory effluent, reclaim remaining silicon-dioxide and purifying waste adopts German import 1.6Mpa autoclave diaphragm filter plant to filter; (2) the above-mentioned waste liquid that obtains is imported the I single-effect evaporator, pour the base fluid in the I single-effect evaporator into base fluid that the base fluid in II single-effect evaporator, the II single-effect evaporator pours in III single-effect evaporator, the III single-effect evaporator and pour the IV single-effect evaporator into, guarantee in the said process liquid level in each single-effect evaporator in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.5Mpa, pressure in the last evaporator is 0.07Mpa, and the steam that feeds temperature then and be 160 ℃ is with concentrating spent liquor; (3) when the concentration of sodium sulfate in the waste liquid reaches 35%, it is delivered to whizzer with sodium sulfate and water centrifugation; (4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 150 ℃, and pressure is 0.55Mpa, promptly gets the powdery industrial anhydrous sodium sulfate, and the hot steam of each single-effect evaporator generation obtains deionized water after condensation simultaneously.
Embodiment 3:
From the precipitated silica factory effluent, extract the method for industrial anhydrous sodium sulfate, may further comprise the steps: (1) filters the precipitated silica factory effluent, reclaim remaining silicon-dioxide and purifying waste adopts German import 1.6Mpa autoclave diaphragm filter plant to filter; (2) the above-mentioned waste liquid that obtains is imported the I single-effect evaporator, pour the base fluid in the I single-effect evaporator into base fluid that the base fluid in II single-effect evaporator, the II single-effect evaporator pours in III single-effect evaporator, the III single-effect evaporator and pour the IV single-effect evaporator into, guarantee in the said process liquid level in each single-effect evaporator in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.45Mpa, pressure in the last evaporator is 0.05Mpa, and the steam that feeds temperature then and be 150 ℃ is with concentrating spent liquor; (3) when the concentration of sodium sulfate in the waste liquid reaches 32%, it is delivered to whizzer with sodium sulfate and water centrifugation; (4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 145 ℃, and pressure is 0.5Mpa, promptly gets the powdery industrial anhydrous sodium sulfate, and the hot steam of each single-effect evaporator generation obtains deionized water after condensation simultaneously.
Embodiment 4:
From the precipitated silica factory effluent, extract the method for industrial anhydrous sodium sulfate, may further comprise the steps: (1) filters the precipitated silica factory effluent, reclaim remaining silicon-dioxide and purifying waste adopts German import 1.6Mpa autoclave diaphragm filter plant to filter; (2) the above-mentioned waste liquid that obtains is imported the I single-effect evaporator, pour the base fluid in the I single-effect evaporator into base fluid that the base fluid in II single-effect evaporator, the II single-effect evaporator pours in III single-effect evaporator, the III single-effect evaporator and pour the IV single-effect evaporator into, guarantee in the said process liquid level in each single-effect evaporator in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.5Mpa, pressure in the last evaporator is 0.06Mpa, and the steam that feeds temperature then and be 155 ℃ is with concentrating spent liquor; (3) when the concentration of sodium sulfate in the waste liquid reaches 34%, it is delivered to whizzer with sodium sulfate and water centrifugation; (4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 150 ℃, and pressure is 0.45Mpa, promptly gets the powdery industrial anhydrous sodium sulfate, and the hot steam of each single-effect evaporator generation obtains deionized water after condensation simultaneously.

Claims (2)

1, a kind of method of extracting industrial anhydrous sodium sulfate from the precipitated silica factory effluent is characterized in that may further comprise the steps:
(1) the precipitated silica factory effluent is filtered, reclaim remaining silicon-dioxide and purifying waste;
(2) the above-mentioned waste liquid that obtains is imported vaporizer, and the liquid level in the control vaporizer in evaporator room on liquid level, the steam that feeds temperature then and be 145-160 ℃ is with concentrating spent liquor;
(3) when the concentration of sodium sulfate in the waste liquid reaches 30-35%, it is delivered to whizzer with sodium sulfate and water centrifugation;
(4) sodium sulfate that obtains in the step (3) is put into moisture eliminator, the temperature in the control moisture eliminator is 140-150 ℃, and pressure is 0.4-0.55Mpa, promptly gets industrial anhydrous sodium sulfate.
2, the method of from the precipitated silica factory effluent, extracting industrial anhydrous sodium sulfate according to claim 1, it is characterized in that: the vaporizer described in the above-mentioned steps (2) is the IV single-effect evaporator, pour the base fluid in the I single-effect evaporator into the II single-effect evaporator, base fluid in the II single-effect evaporator is poured the III single-effect evaporator into, base fluid in the III single-effect evaporator is poured the IV single-effect evaporator into, guarantee in the said process liquid level in each single-effect evaporator in evaporator room on liquid level, pressure in the control I single-effect evaporator is 0.4-0.5Mpa, and the pressure in the last evaporator is 0.04-0.07Mpa.
CNB2006101023472A 2006-12-28 2006-12-28 Method of extracting industrial anhydrous sodium sulfate from waste water in silicone dioxide production using precipitation method Expired - Fee Related CN100513312C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102001690A (en) * 2010-11-24 2011-04-06 陈君华 Method for preparing industrial anhydrous sodium sulfate
CN102689999A (en) * 2012-04-25 2012-09-26 浙江省海洋开发研究院 Resourceful treatment method for silica gel waste water
CN107921371A (en) * 2015-07-28 2018-04-17 罗地亚经营管理公司 method for recycling sodium sulphate

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030342B (en) * 2010-10-26 2012-09-19 天脊煤化工集团股份有限公司 Method and device for recovering anhydrous sodium sulfate from hydroxy benzotriazole production waste liquor

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102001690A (en) * 2010-11-24 2011-04-06 陈君华 Method for preparing industrial anhydrous sodium sulfate
CN102001690B (en) * 2010-11-24 2012-07-25 陈君华 Method for preparing industrial anhydrous sodium sulfate
CN102689999A (en) * 2012-04-25 2012-09-26 浙江省海洋开发研究院 Resourceful treatment method for silica gel waste water
CN107921371A (en) * 2015-07-28 2018-04-17 罗地亚经营管理公司 method for recycling sodium sulphate

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