CN108946678A - A kind of processing method of industrial chlorinations salt - Google Patents
A kind of processing method of industrial chlorinations salt Download PDFInfo
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- CN108946678A CN108946678A CN201810145589.2A CN201810145589A CN108946678A CN 108946678 A CN108946678 A CN 108946678A CN 201810145589 A CN201810145589 A CN 201810145589A CN 108946678 A CN108946678 A CN 108946678A
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- salt
- sulfur trioxide
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- industrial chlorinations
- chlorinations
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/46—Compounds containing sulfur, halogen, hydrogen, and oxygen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of processing methods of industrial chlorinations salt, comprising the following steps: industrial chlorinations salt and sulfur trioxide are reacted at 80~200 DEG C, obtain chlorosulfonate.The present invention uses sulfur trioxide as strong oxidizer at high temperature, and extends residence time of material, converts chlorosulfonate for abraum salt, while carrying out oxidation processes removing to the organic matter in abraum salt during reaction.The technique can not only eliminate influence of the industrial chlorinations salt as solid waste to environment, can also realize the recycling of industrial chlorinations salt by-product, realize circular economy, do not have secondary pollution in production, the production requirement of green chemical industry may be implemented.Industrial by-product industrial chlorinations salt is turned waste into wealth, there is highly important realistic meaning and good social benefit and environmental benefit, has great strategic significance to Resources for construction economizing type and friendly environment society.
Description
Technical field
The present invention relates to chemical industrial waste object post-processing technology field more particularly to a kind of processing methods of industrial chlorinations salt.
Background technique
Major part chemical company can all generate high-salt wastewater in process of production at present, can be obtained by a series of processing
To the by-product industrial chlorinations salt for containing a small amount of organic matter, this part salt is difficult to be effectively addressed and utilize, and can only be used as dangerous waste
It handles, not only not any economic value, but also higher processing cost can be consumed, about 3000-5000 yuan/ton of expense.
The main means of processing dangerous waste are exactly to fill at present, if leakage accidentally, will cause secondary pollution.
Only a small number of chemical companies can further refine the part salt at present, improve the content of salt, but
It is that product that current technique obtains can't be directly as the raw material of downstream product.Such as by hot-blast oxidation method, treated
Its content of industrial chlorinations salt significantly improves, but cannot reach the requirement of chlorine industry, can only be used as snow-melting agent, economic value
It is lower, and exhaust gas generation is had in the process.So how industrial chlorinations salt is converted into other useful chemical products is mesh
Preceding technical problem urgently to be solved.
And conventional chlorate is reacted with sulfur trioxide, the method for generating sulfur dioxide, chlorine and sodium sulphate can generate packet
Problem is wrapped up in, the chlorosulfonate that sodium chloride and sulfur trioxide reaction generate can be wrapped in the surface of sodium chloride, and then hinder three oxidations
Sulphur further with chlorination reactant salt, causes reaction to be not thorough, and yield is lower, can be containing a large amount of not anti-in obtained chlorosulfonate
The chlorate answered leads to rejected product occur, and obtained product is not able to satisfy national standard.And the process for increasing grinding can then produce
Fecula dirt, and increase post-processing difficulty.
Summary of the invention
In view of this, having the technical problem to be solved in the present invention is that providing a kind of processing method of industrial chlorinations salt
Higher yield, and obtained product can direct industrial utilization.
In order to solve the above technical problems, the present invention provides a kind of processing methods of industrial chlorinations salt, comprising the following steps:
Industrial chlorinations salt and sulfur trioxide are reacted at 80~200 DEG C, obtain chlorosulfonate.
The present invention provides the sides that the industrial chlorinations salt that a kind of pair of chemical company generates in process of production is post-processed
Method is efficiently recycled industrial waste salt by adjusting suitable technique and parameter, can not only eliminate to environment
Influence, and industrial by-product can be made to obtain secondary use, realize circular economy, generate very big industrial value.
The equation of above-mentioned reaction is as follows:
SO3(l/q)+Cl-→SO3Cl-
The industrial chlorinations salt includes any one or a few in sodium chloride, potassium chloride, ammonium chloride and magnesium chloride, and
Organic matter.
In the present invention, the organic matter can be aromatic series or aliphatic category organic matter.
Wherein, the content of the organic matter is 0-3%, more preferably 0.1%~2.5%, of the invention certain specific
In embodiment, the content is 2%.Above-mentioned content is mass content.
The present invention is to the source of above-mentioned industrial chlorinations salt and is not particularly limited, the content of organics that general chemical company generates
0~3% chlorate.
The sulfur trioxide can be gaseous state or liquid.
Since the reaction of chlorate and sulfur trioxide is that strong exothermal reaction can pass through when using liquid sulphur trioxide
The state of sulfur trioxide changes (liquid to gaseous vaporization) and effectively removes the heat that reaction generates, and can effectively control anti-
The temperature of charge in device is answered, sharply temperature rise is avoided.
When using gaseous sulfur trioxide, heat can effectively be removed by outer circulation mode, it can also be by controlling chlorination
Salt and sulfur trioxide add rate to control the heat generated in the reacton time.
The volumetric concentration of the sulfur trioxide is 50%~100%, more preferable 50%~99%.
Method provided by the invention is not high to the purity requirement of sulfur trioxide, when sulfur trioxide purity is 50%~100%
It can meet the requirements.When sulfur trioxide concentration is lower, such as the sulphur-containing exhaust gas of enterprise, sulfur trioxide concentration is generally 50%~
60%, also contain a large amount of inert gas impurity, these inert gases can't participate in reacting, can be up to standard after vent gas treatment
Discharge.The vent gas treatment can be the method for water absorption+Alkali absorption well known in the art.Therefore above-mentioned place provided by the invention
Reason method, can be with the sulphur-containing exhaust gas of reuse enterprise, and not only abraum salt has obtained recycling, but also also reduces the row of sulphur-containing gas
It puts, achieves many things at one stroke.
Specifically, the sulphur-containing exhaust gas may include sulfur trioxide, sulfur dioxide, air, aqueous vapor etc. will be described before reaction
Sulphur-containing exhaust gas can be reacted through being dried, and reaction system preferably includes exhaust gas processing device, the exhaust gas processing device
It can be desulphurization system well known in the art, unreacted gas is post-processed.When using the sulfur trioxide of low-purity,
The inert gas for not participating in reaction can all enter exhaust treatment system, the qualified discharge after simple process.
The mass ratio of the industrial chlorinations salt and sulfur trioxide is preferably (50~100): (50~200), more preferably (80
~100): (80~100).
The temperature of the reaction is preferably 80~200 DEG C, and more preferably 105~180 DEG C.Time is preferably 1-100min,
More preferably 5-50min.
For the present invention by the restriction of above-mentioned parameter, the product chlorosulfonate that reaction can be carried out quickly, while be obtained is liquid
State or molten state solve the problems, such as chlorosulfonate to the package of sodium chloride, therefore to the partial size of abraum salt without specific requirement, also with regard to nothing
Grinding pretreatment need to be carried out to abraum salt, without being ground during the reaction to chlorate, fundamentally solved
Grind a series of vent gas treatments of bring and operating environment, such as dust problem.
Further, the present invention utilizes sulfur trioxide in the strong oxidizing property of the condition of high temperature, during the reaction in abraum salt
Organic matter carry out oxidation processes removing, and then ensure that the quality of chlorosulfonate.
In addition, the chlorosulfonate formed is liquid, it is also convenient for the circulation conveying of material, and is convenient for the shifting of insoluble impurities
It removes, the chlorosulfonate of high-quality can be obtained.
Therefore after reaction, it is filtered to remove impurity, is post-processed very simple.
Compared with prior art, the present invention provides a kind of processing methods of industrial chlorinations salt, comprising the following steps: industry
Chlorate and sulfur trioxide are reacted at 80~200 DEG C, obtain chlorosulfonate.The present invention uses sulfur trioxide at high temperature
As strong oxidizer, and extend residence time of material, convert chlorosulfonate for abraum salt, while to useless during reaction
Organic matter in salt carries out oxidation processes removing.The technique can not only eliminate shadow of the industrial chlorinations salt as solid waste to environment
It rings, can also realize the recycling of industrial chlorinations salt by-product, realize circular economy, do not have secondary pollution in production, it can be with
Realize the production requirement of green chemical industry.Industrial by-product industrial chlorinations salt is turned waste into wealth, there is highly important realistic meaning and good
Good social benefit and environmental benefit, has great strategic significance to Resources for construction economizing type and friendly environment society.
Specific embodiment
In order to further illustrate the present invention, below with reference to embodiment to the processing method of industrial chlorinations salt provided by the invention
It is described in detail.
Multiple-effect sodium chloride, multiple-effect potassium chloride, multiple-effect magnesium chloride and the multiple-effect ammonium chloride of the following embodiments of the present invention are to adopt
The high-salt wastewater that synthetic workshop generates is concentrated to give with multiple-effect evaporation or MVR equipment.
Embodiment 1
It takes 15.65g multiple-effect sodium chloride (containing 0.12% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 100 DEG C, and the sulfur trioxide that gaseous state 99.9% is then slowly passed through into reaction unit is stirred to react, three oxidations
The rate that is passed through of sulphur is subject to the temperature of material in reaction unit and is increased without significant, the average addition rate of laboratory sulfur trioxide
For 0.5g/min, it is stirred to react.When the quality for being passed through sulfur trioxide is 21.38g, chlorosulfonic acid sodium 37.02g is obtained.
Chlorosulfonic acid sodium is decomposed into sodium sulphate to detect, counter after testing to push away, chlorosulfonic acid sodium purity obtained is 98%,
Additionally containing 1.2% sodium chloride and 0.8% sodium pyrosulfate.
Wherein, sodium chloride is determined by chloride test；Sodium pyrosulfate is determined by preparing aqueous solution, detection hydrogen ion.
Embodiment 2
It takes 15.58g multiple-effect sodium chloride (containing 0.97% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 150 DEG C, and the sulfur trioxide that gaseous state 50.6% is then slowly passed through into reaction unit is stirred to react, three oxidations
The rate that is passed through of sulphur is subject to the temperature of material in reaction unit and is increased without significant, the average addition rate of laboratory sulfur trioxide
For 1.1g/min, it is stirred to react.When the quality for being passed through sulfur trioxide is 21.11g, chlorosulfonic acid sodium substance 36.54g is obtained.
Chlorosulfonic acid sodium is decomposed into sodium sulphate to detect, counter after testing to push away, obtained chlorosulfonic acid sodium purity is
98.43%, additionally containing 0.98% sodium chloride and 0.59% sodium pyrosulfate.
Embodiment 3
It takes 15.19g multiple-effect sodium chloride (containing 2.1% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 180 DEG C, and the sulfur trioxide that gaseous state 80% is then slowly passed through into reaction unit is stirred to react, sulfur trioxide
The rate that is passed through be subject to the temperature of material in reaction unit and increased without significant, the average addition rate of laboratory sulfur trioxide is
0.87g/min is stirred to react.When the quality for being passed through sulfur trioxide is 20.35g, chlorosulfonic acid sodium substance 35.21g is obtained.
Chlorosulfonic acid sodium is decomposed into sodium sulphate to detect, counter after testing to push away, reacting chlorosulfonic acid sodium purity obtained is
99.12%, additionally containing 0.79% sodium chloride and 0.09% sodium pyrosulfate.
Embodiment 4
It takes 15.88g multiple-effect sodium chloride (containing 2.8% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 130 DEG C, and 99% sulfur trioxide that liquid is then added into reaction unit is stirred to react, the sulfur trioxide of gasification
By being returned in reaction unit after condensing tube condensation, in entire reaction process control reaction unit in temperature of charge 130 ± 3
DEG C, when the quality for being passed through sulfur trioxide is 21.11g, obtain chlorosulfonic acid sodium substance 36.54g.
Chlorosulfonic acid sodium is decomposed into sodium sulphate to detect, counter after testing to push away, chlorosulfonic acid sodium purity obtained is
97.12%, additionally containing 0.43% sodium chloride and 2.45% sodium pyrosulfate.
Embodiment 5
It takes 15.59g multiple-effect potassium chloride (containing 1.17% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 150 DEG C, and the sulfur trioxide that gaseous state 50.6% is then slowly passed through into reaction unit is stirred to react, three oxidations
The rate that is passed through of sulphur is subject to the temperature of material in reaction unit and is increased without significant, the average addition rate of laboratory sulfur trioxide
For 1.1g/min, it is stirred to react.When the quality for being passed through sulfur trioxide is 16.55g, chlorosulfonic acid potassium substance 31.96g is obtained.
Chlorosulfonic acid potassium is decomposed into potassium sulfate to detect, counter after testing to push away, obtained chlorosulfonic acid potassium purity is
98.57%, additionally containing 0.91% potassium chloride and 0.52% potassium pyrosulfate.Meet national standard.
Embodiment 6
It takes 22.1g multiple-effect magnesium chloride (containing 0.11% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 150 DEG C, and the sulfur trioxide that gaseous state 50.6% is then slowly passed through into reaction unit is stirred to react, three oxidations
The rate that is passed through of sulphur is subject to the temperature of material in reaction unit and is increased without significant, the average addition rate of laboratory sulfur trioxide
For 1.03g/min, it is stirred to react.When the quality for being passed through sulfur trioxide is 37.1g, the substance 59.17g of chlorosulfonic acid magnesium is obtained.
Chlorosulfonic acid magnesium is decomposed into magnesium sulfate to detect, counter after testing to push away, obtained chlorosulfonic acid magnesium purity is
97.61%, additionally containing 1.31% magnesium chloride and 1.08% pyrosulfuric acid magnesium.
Embodiment 7
It takes 14.5g multiple-effect ammonium chloride (containing 0.47% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 95 DEG C (due to starting to decompose when ammonium chloride is heated to 100 DEG C, so the reaction temperature of the present embodiment control is 95
DEG C), the sulfur trioxide that gaseous state 99% is then slowly passed through into reaction unit is stirred to react, sulfur trioxide be passed through rate with
In reaction unit the temperature of material without significant increase subject to, the average addition rate of laboratory sulfur trioxide is 0.5g/min, is stirred
Mix reaction.When the quality for being passed through sulfur trioxide is 21.58g, the substance 36.0g of chlorosulfonic acid ammonium is obtained.
Chlorosulfonic acid ammonium is decomposed into ammonium sulfate to detect, counter after testing to push away, obtained chlorosulfonic acid ammonium purity is
98.74%, additionally containing 0.71% ammonium chloride and 0.55% ammonium pyrosulfate.
Comparative example 1
It takes 15.2g multiple-effect sodium chloride (containing 0.12% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 70 DEG C, and the sulfur trioxide that gaseous state 99% is then slowly passed through into reaction unit is stirred to react, sulfur trioxide
The rate that is passed through be subject to the temperature of material in reaction unit and increased without significant, the average addition rate of laboratory sulfur trioxide is
1.1g/min is stirred to react.After the quality for being passed through sulfur trioxide is 6.3g, a large amount of sulfur trioxide enters tail gas absorption system
System, the material state in reaction unit at this time is hard solid-state, and stirring is obstructed.Stop experiment at this time, it will be in reaction unit
Material be decomposed into sodium sulphate and detected, counter after testing to push away, obtained chlorosulfonic acid sodium purity is 13.82%, is additionally contained
There are 83.18% sodium chloride and 3% sodium pyrosulfate.
Comparative example 2:
It takes 15.18g multiple-effect sodium chloride (containing 0.12% organic matter) into reaction unit, makes reaction unit using oil bath pan
Temperature maintains 200 DEG C, and the sulfur trioxide that gaseous state 99% is then slowly passed through into reaction unit is stirred to react, sulfur trioxide
The rate that is passed through be subject to the temperature of material in reaction unit and increased without significant, the average addition rate of laboratory sulfur trioxide is
0.6g/min is stirred to react.When reaction temperature is 200 DEG C, there is the generation of yellow green gas in reaction unit, show that the reaction exists
It is cracked while reaction, generates chlorine and sulfur dioxide, which can mix with sulfur trioxide and enter gas
Body collection system influences the utilization of chlorine and sulfur dioxide.
By above-described embodiment and comparative example it is found that the processing method provided by the present invention, conversion ratio with higher.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (8)
1. a kind of processing method of industrial chlorinations salt, comprising the following steps:
Industrial chlorinations salt and sulfur trioxide are reacted at 80~200 DEG C, obtain chlorosulfonate.
2. processing method according to claim 1, which is characterized in that the industrial chlorinations salt include sodium chloride, potassium chloride,
Any one or a few and organic matter in ammonium chloride and magnesium chloride.
3. processing method according to claim 2, which is characterized in that the content of the organic matter is 0~3%.
4. processing method according to claim 1, which is characterized in that the sulfur trioxide is gaseous state or liquid.
5. processing method according to claim 1, which is characterized in that the volumetric concentration of the sulfur trioxide be 50%~
100%.
6. processing method according to claim 1, which is characterized in that the mass ratio of the industrial chlorinations salt and sulfur trioxide
For (50~100): (50~200).
7. processing method according to claim 1, which is characterized in that the temperature of the reaction is 105~180 DEG C.
8. processing method according to claim 1, which is characterized in that the time of the reaction is 1-100min.
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| CN201810145589.2A CN108946678A (en) | 2018-02-12 | 2018-02-12 | A kind of processing method of industrial chlorinations salt |
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| CN201810145589.2A CN108946678A (en) | 2018-02-12 | 2018-02-12 | A kind of processing method of industrial chlorinations salt |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB522209A (en) * | 1938-12-07 | 1940-06-12 | Du Pont | Improvements in or relating to the manufacture of chlorosulphonates |
| US2218729A (en) * | 1938-10-20 | 1940-10-22 | Du Pont | Process for the production of chlorosulphonates |
-
2018
- 2018-02-12 CN CN201810145589.2A patent/CN108946678A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2218729A (en) * | 1938-10-20 | 1940-10-22 | Du Pont | Process for the production of chlorosulphonates |
| GB522209A (en) * | 1938-12-07 | 1940-06-12 | Du Pont | Improvements in or relating to the manufacture of chlorosulphonates |
Non-Patent Citations (4)
| Title |
|---|
| W. L. FIELDER，等: "Reactions of NaCI with Gaseous SO3 , SO2 , and O2", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》 * |
| 佟玉衡: "《实用废水处理技术》", 30 November 1998 * |
| 刘少武，等: "《硫酸工作手册》", 30 April 2001 * |
| 辽宁省石油化学工业厅: "《辽宁化工产品大全》", 31 December 1992 * |
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