CN112225233A - A kind of method for preparing sodium bisulfate - Google Patents

A kind of method for preparing sodium bisulfate Download PDF

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Publication number
CN112225233A
CN112225233A CN202011162949.3A CN202011162949A CN112225233A CN 112225233 A CN112225233 A CN 112225233A CN 202011162949 A CN202011162949 A CN 202011162949A CN 112225233 A CN112225233 A CN 112225233A
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China
Prior art keywords
sodium
hydrogen peroxide
solution
sodium bisulfite
preparing
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CN202011162949.3A
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Chinese (zh)
Inventor
陈志敏
张翠红
张颖
景银兰
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Taiyuan Institute of Technology
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Taiyuan Institute of Technology
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Priority to CN202011162949.3A priority Critical patent/CN112225233A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D5/00Sulfates or sulfites of sodium, potassium or alkali metals in general
    • C01D5/02Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

本发明涉及无机化工领域,具体涉及一种制备硫酸氢钠的方法;以硫代硫酸钠或亚硫酸氢钠为原料,以过氧化氢为氧化剂,通过氧化还原反应,制备硫酸氢钠;本发明方法采用的原料为硫代硫酸钠或亚硫酸氢钠是常见的无机盐,无腐蚀性,而过氧化氢是一种对环境友好的清洁氧化剂,避免了以强酸、强碱为原料对设备产生的腐蚀,采用本发明制备方法安全性高,且方法操作过程简单,因此可望成为硫酸氢钠的一种清洁制备方法。The invention relates to the field of inorganic chemical industry, in particular to a method for preparing sodium bisulfate; using sodium thiosulfate or sodium bisulfite as a raw material, using hydrogen peroxide as an oxidant, and preparing sodium bisulfate through a redox reaction; the present invention The raw materials used in the method are sodium thiosulfate or sodium bisulfite, which are common inorganic salts and are non-corrosive, while hydrogen peroxide is an environmentally friendly cleaning oxidant, which avoids the generation of equipment by using strong acids and alkalis as raw materials. The preparation method of the present invention has high safety and simple operation process, so it is expected to be a clean preparation method of sodium hydrogen sulfate.

Description

Method for preparing sodium bisulfate
Technical Field
The invention relates to the field of inorganic chemical industry, in particular to a method for preparing sodium bisulfate.
Background
Sodium bisulfate is an important inorganic chemical product, can be used as a cosolvent, a dyeing assistant, a disinfectant, a preservative, a cleaning agent and a catalyst, and can be used for preparing sulfate, sodium alum and the like.
The preparation method of the sodium bisulfate mainly comprises the following steps:
sodium hydroxide and sulfuric acid are used as raw materials. The reaction principle is as follows:
NaOH+H2SO4→NaHSO4+H2O
sodium sulfate and sulfuric acid are used as raw materials. The reaction principle is as follows:
Na2SO4+H2SO4→2NaHSO4
sodium chloride and sulfuric acid are used as raw materials. The reaction principle is as follows:
NaCl+H2SO4→NaHSO4+HCl
these methods all use strong acid and strong base, and are very corrosive to equipment.
Disclosure of Invention
The invention provides a method for preparing sodium bisulfate, which aims to solve the problem that strong acid and strong base are adopted during the preparation of sodium bisulfate in the prior art, so that equipment is seriously corroded.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: sodium thiosulfate or sodium bisulfite is used as a raw material, and hydrogen peroxide is used as an oxidant to prepare sodium bisulfate through oxidation-reduction reaction.
The reaction principle is as follows:
Na2S2O3+4H2O2→2NaHSO4+3H2O
NaHSO3+H2O2→NaHSO4+H2O
further, the method of the invention adopts the following specific steps:
hydrogen peroxide was added to a round bottom flask equipped with a reflux condenser and a constant pressure dropping funnel. Dissolving sodium thiosulfate or sodium bisulfite in water to obtain a solution. Sodium thiosulfate or sodium bisulfite solution was added dropwise to the flask with stirring.
When the raw material is sodium bisulfite, the obtained reaction solution is poured into an evaporating dish, is put on a boiling water bath for evaporation, is concentrated until no bubbles are generated, is put into a drier for cooling to room temperature, and is transferred into a container for sealed storage.
When the raw material is sodium thiosulfate, the obtained reaction solution is heated on a boiling water bath for 1 hour, cooled to room temperature, filtered, taken out, poured into an evaporating dish, placed on the boiling water bath for evaporation, concentrated until no bubbles are generated, and then placed into a dryer for cooling to room temperature. And (4) moving the product into a container for sealing and storing.
In the specific steps, the reaction liquid is evaporated on a boiling water bath, and the concentration degree is bubble-free, which is the key point of the method of the invention, and the collected sodium bisulfate has high yield and high content. In addition, the order of adding the sodium thiosulfate or sodium bisulfite solution to the hydrogen peroxide solution is also critical in the preparation method.
Preferably, the sodium thiosulfate or sodium bisulfite solution is dripped into the hydrogen peroxide solution in a stirring and dripping manner, the dripping speed is 1 drop in 4-5 seconds, and stirring is continued for 10 minutes after dripping is finished.
Further, the mass ratio of hydrogen peroxide to sodium thiosulfate used is greater than 4: 1.
Further, the amount of hydrogen peroxide to sodium bisulfite used is greater than 1: 1.
Compared with the prior art, the invention has the following beneficial effects:
the raw materials adopted by the method are sodium thiosulfate or sodium bisulfite which is common inorganic salt and has no corrosiveness, and the hydrogen peroxide is an environment-friendly clean oxidant, so that the corrosion of equipment caused by strong acid and strong alkali is avoided.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
A50 mL round-bottom flask equipped with a water bath, reflux condenser and constant pressure dropping funnel was charged with 10mL of 30% by mass hydrogen peroxide. Weighing 4.9767gNa2S2O3·5H2O was dissolved in 10mL of deionized water to make a solution. Starting stirring, dropwise adding the sodium thiosulfate solution into the flask at the speed of 1 drop every 4-5 seconds, and continuing stirring for 10 minutes after the addition is finished. Heat in a boiling water bath for 1 hour. Cooled to room temperature and filtered with suction. The filtrate is poured into an evaporating dish inEvaporating on boiling water bath, and concentrating until no bubbles are generated. The mixture was cooled to room temperature in a desiccator. Weighed to give 5.1334g of colorless crystals in 92.70% yield (in NaHSO)4·H2And O is calculated). The content of NaHSO is determined according to HG/T4516-4·H2The O content was 98.58%.
Example 2
A50 mL round-bottom flask equipped with a reflux condenser and a constant pressure dropping funnel was charged with 6mL of 30% by mass hydrogen peroxide. Weighing 5.2154g NaHSO3Dissolved in 10mL of deionized water to prepare a solution. Starting stirring, dropwise adding the sodium bisulfite solution into the flask at the speed of 1 drop every 4-5 seconds, and continuing stirring for 10 minutes after the addition is finished. Pouring the reaction solution into an evaporating dish, evaporating on a boiling water bath, and concentrating until no bubbles are generated. The mixture was cooled to room temperature in a desiccator. Weighed to give 6.5066g of colorless crystals, yield 94.02% (as NaHSO)4·H2And O is calculated). The content of NaHSO is determined according to HG/T4516-4·H2The O content was 91.16%.

Claims (5)

1.一种制备硫酸氢钠的方法,其特征在于,以硫代硫酸钠或亚硫酸氢钠为原料,以过氧化氢为氧化剂,通过氧化还原反应,制备硫酸氢钠。1. a method for preparing sodium bisulfate, is characterized in that, with sodium thiosulfate or sodium bisulfite as raw material, with hydrogen peroxide as oxidant, by redox reaction, prepare sodium bisulfate. 2.根据权利要求1所述的一种制备硫酸氢钠的方法,其特征在于,当原料选用亚硫酸氢钠时,制备硫酸氢钠具体步骤为将亚硫酸氢钠溶液滴加到过氧化氢溶液中,所得反应液倒入蒸发皿中置于沸水浴蒸发、浓缩至无气泡产生,置于干燥器中冷却至室温得到硫酸氢钠;2. a kind of method for preparing sodium bisulfite according to claim 1, is characterized in that, when raw material selects sodium bisulfite, the concrete steps of preparing sodium bisulfite are that sodium bisulfite solution is added dropwise to hydrogen peroxide In the solution, the obtained reaction solution is poured into an evaporating dish, placed in a boiling water bath for evaporation, concentrated until no bubbles are generated, placed in a desiccator and cooled to room temperature to obtain sodium bisulfate; 当原料选用硫代硫酸钠时,制备硫酸氢钠具体步骤为将亚硫酸氢钠溶液滴加到过氧化氢溶液中,在沸水浴加热1小时,冷至室温,抽滤,取其滤液倒入蒸发皿中置于沸水浴上蒸发、浓缩至无气泡产生,置于干燥器中冷却至室温得到硫酸氢钠。When sodium thiosulfate is selected as the raw material, the specific steps for preparing sodium bisulfate are as follows: adding sodium bisulfite solution dropwise to the hydrogen peroxide solution, heating in a boiling water bath for 1 hour, cooling to room temperature, suction filtration, taking the filtrate and pouring it into the hydrogen peroxide solution. Place in an evaporating dish on a boiling water bath to evaporate and concentrate until no bubbles are generated, and place in a desiccator to cool to room temperature to obtain sodium bisulfate. 3.根据权利要求2所述的一种制备硫酸氢钠的方法,其特征在于,所述硫代硫酸钠或亚硫酸氢钠溶液滴加至过氧化氢溶液中时采用边搅拌边滴入的方式,滴加的速度为4-5秒1滴,滴加完后继续搅拌10分钟。3. a kind of method for preparing sodium bisulfate according to claim 2, is characterized in that, adopts the dripping while stirring when described sodium thiosulfate or sodium bisulfite solution are dripped in the hydrogen peroxide solution method, the speed of dripping is 1 drop in 4-5 seconds, and the stirring is continued for 10 minutes after the dripping. 4.根据权利要求1或2所述的一种制备硫酸氢钠的方法,其特征在于,所用过氧化氢与硫代硫酸钠的物质的量之比大于4∶1。4. a kind of method for preparing sodium bisulfate according to claim 1 and 2 is characterized in that, the ratio of the amount of substance of hydrogen peroxide used and sodium thiosulfate is greater than 4: 1. 5.根据权利要求1或2所述的一种制备硫酸氢钠的方法,其特征在于,所用过氧化氢与亚硫酸氢钠的物质的量之比大于1∶1。5. a kind of method for preparing sodium bisulfite according to claim 1 and 2, is characterized in that, the ratio of the amount of substance of hydrogen peroxide used and sodium bisulfite is greater than 1: 1.
CN202011162949.3A 2020-10-27 2020-10-27 A kind of method for preparing sodium bisulfate Pending CN112225233A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7045110B1 (en) * 2004-11-17 2006-05-16 Poly Systems Usa, Inc. High yield co-production of anhydrous hydrogen bromide and sodium bisulfate
CN103408040A (en) * 2013-07-02 2013-11-27 中南大学 Method for preparing sodium hydrogen sulfate through microwave radiation
TW201420514A (en) * 2012-11-19 2014-06-01 I-Fang Chen Method of using sulfur-containing reductant to treat hydrogen peroxide in sulfuric acid aqueous solution
CN106044801A (en) * 2016-05-26 2016-10-26 中国中轻国际工程有限公司 Process for producing sodium bisulfate from sodium sulfate and sodium chloride containing carrier

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7045110B1 (en) * 2004-11-17 2006-05-16 Poly Systems Usa, Inc. High yield co-production of anhydrous hydrogen bromide and sodium bisulfate
TW201420514A (en) * 2012-11-19 2014-06-01 I-Fang Chen Method of using sulfur-containing reductant to treat hydrogen peroxide in sulfuric acid aqueous solution
CN103408040A (en) * 2013-07-02 2013-11-27 中南大学 Method for preparing sodium hydrogen sulfate through microwave radiation
CN106044801A (en) * 2016-05-26 2016-10-26 中国中轻国际工程有限公司 Process for producing sodium bisulfate from sodium sulfate and sodium chloride containing carrier

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱洪法: "《精细化工常用原材料手册》", 31 December 2003, 金盾出版社 *

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