CN210065188U - Device for preparing carbonyl sulfide gas - Google Patents
Device for preparing carbonyl sulfide gas Download PDFInfo
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- CN210065188U CN210065188U CN201920726269.6U CN201920726269U CN210065188U CN 210065188 U CN210065188 U CN 210065188U CN 201920726269 U CN201920726269 U CN 201920726269U CN 210065188 U CN210065188 U CN 210065188U
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Abstract
The utility model discloses a gaseous device of preparation carbonyl sulfide, the device are met through the pipeline by reation kettle, raw materials dropwise add jar A, raw materials dropwise add jar B, condenser, desicator, compressor, product bottle and form. The utility model discloses can show the efficiency that improves ammonium thiocyanate and sulphuric acid reaction with the reaction mode of ammonium thiocyanate and concentrated sulfuric acid dropwise add simultaneously, reduce the formation of impurity, improve the yield of carbonyl sulfide product by a wide margin, the product yield can reach more than 93%.
Description
Technical Field
The utility model belongs to a method and a device for preparing carbonyl sulfide gas, in particular to a method and a device for preparing carbonyl sulfide gas by adopting a mode of dropwise adding ammonium thiocyanate and concentrated sulfuric acid simultaneously.
Background
Carbonyl sulfide, also known as carbonyl sulfide, is a gas widely used in the production of medicines, pesticides and other chemical products, has been used as a fumigant for grains all the time, has the characteristics of moderate toxicity, easy degradation and the like, and is also an important raw material for synthesizing thiocarbamate pesticides and insecticides. In recent years, high purity carbon oxysulfide has been used in integrated circuit etching processes, and the trend is strong.
Currently, methods for preparing carbonyl sulfide are classified into a dry method and a wet method, and the difference is whether the synthesis reaction is performed in an aqueous solution.
① Dry Process for producing carbonyl sulfide is the reaction of elemental sulfur with carbon monoxide,
CO+S→COS
the method needs to be carried out under high temperature, a catalyst is needed in the reaction process, and the raw material carbon monoxide is a high-cost toxic gas, so that more dangerous factors exist in the production process.
② A representative process for the wet production of carbonyl sulfide is the ammonium thiocyanate process,
NH4SCN+H2SO4→COS+（NH4）2SO4
the method has the advantages of mild reaction conditions, few dangerous factors in the reaction process and low raw material cost. However, since this method is carried out in an aqueous solution, side reactions occur in the reaction process, and impurities such as sulfur, carbon dioxide, and hydrogen sulfide are produced in a large amount, so that the yield can be maintained only at about 80%.
Disclosure of Invention
In order to overcome the defects of low yield and more impurities in the wet-method production of the carbonyl sulfide, the utility model aims to provide a method for preparing the carbonyl sulfide gas.
The utility model discloses purpose technical solution does:
the utility model provides a gaseous device of preparation carbonyl sulfide, is formed its characterized in that by reation kettle 1, raw materials dropwise add jar A, raw materials dropwise add jar B, condenser, desicator, compressor, product bottle meet through the pipeline: the reation kettle top meet with raw materials dropwise add jar A, raw materials dropwise add jar B respectively through the pipeline, raw materials dropwise add jar A, raw materials dropwise add jar B bottom are equipped with the valve, reation kettle on connect thermometer, manometer and acidimeter respectively, the export tube coupling of condenser entry and reation kettle, desicator entry meet with the condenser export, the desicator export meets with the compressor entry, the compressor export meet with the product bottle.
The dryer is filled with anhydrous calcium chloride.
Compared with the prior art, the utility model have following advantage: the method can obviously improve the reaction efficiency of ammonium thiocyanate and sulfuric acid, reduce the generation of impurities, and greatly improve the yield of the carbon oxysulfide product, wherein the product yield can reach more than 93 percent.
Drawings
FIG. 1 is a process flow diagram of the present invention.
In the figure: 1. the system comprises a reaction kettle, 2 raw material dripping tanks A and 3, raw material dripping tanks B and 4, a condenser, 5, a thermometer, 6, a pressure gauge, 7, an acidimeter, 8, a dryer, 9, a compressor, 10 and a product bottle.
Detailed Description
The embodiments are described below with reference to the accompanying drawings:
gaseous device of preparation carbonyl sulfide is met through the pipeline by reation kettle 1, raw materials dropwise add jar A2, raw materials dropwise add jar B3, condenser 4, desicator 8, compressor 9, product bottle 10 and forms, reation kettle 1 top meet with raw materials dropwise add jar A2, raw materials dropwise add jar B3 respectively through the pipeline, raw materials dropwise add jar A2, raw materials dropwise add jar B3 bottom are equipped with the valve, reation kettle 1 on connect thermometer 5, manometer 5 and acidimeter 5 respectively, condenser 4 entry and reation kettle 1's outlet pipe connection, 8 entrys of desicator meet with the export of condenser 4, 8 exports of desicator meet with the 9 entry of compressor, 9 exports of compressor meet with product bottle 10.
The drier 8 is filled with anhydrous calcium chloride.
The utility model discloses a following step preparation carbonyl sulfide gas:
① adding 65% sulphuric acid into the reaction kettle 1;
② dropping the prepared ammonium thiocyanate solution with the concentration of 65 percent into a raw material dropping tank A2;
③ adding 93% sulfuric acid into the material dripping tank B3;
④ preheating the reaction kettle 1 to 50-70 ℃, and starting stirring;
⑤ opening the valve at the bottom of the material dropping tank A2, dropping ammonium thiocyanate solution into the reaction kettle 1 for reaction;
⑥ and opening the valve at the bottom of the raw material dropping tank B3, and dropping concentrated sulfuric acid into the reaction kettle 1 for reaction.
⑦, controlling the temperature of the reaction kettle 1 to be 50-70 ℃, controlling the acidity of the reaction kettle 1 to be 55-65% and controlling the pressure of the reaction kettle 1 to be 0-0.2 MPa in the reaction process;
⑧, dehydrating the generated carbonyl sulfide gas through a condenser 4, and drying the gas in a dryer 8;
⑨ the dried gas is filled into the cylinder 10 by the compressor 9.
The method has the advantages that the batch charging amount of the sulfuric acid participating in the reaction is divided into two parts, one part is diluted and put into the reaction kettle 1 in advance for reaction, and the other part is replenished in the reaction process, so that the concentration of the sulfuric acid in the reaction kettle 1 is kept in a stable range in the synthesis reaction process, and the reaction yield is greatly improved.
In step ⑥, concentrated sulfuric acid is added dropwise, and the mass feed ratio of the concentrated sulfuric acid to the sulfuric acid filled in the reaction kettle 1 is 1: 2.
In step ⑧, the condenser 4 is at a temperature of-5 deg.C, and the dryer 8 is filled with anhydrous calcium chloride.
Example 1
①, diluting 2/3 of concentrated sulfuric acid with theoretical feeding amount to 65% of concentration, adding the diluted concentrated sulfuric acid into the reaction kettle 1, adding a 65% solution prepared by 25kg of ammonium thiocyanate into a raw material dripping tank A2, and adding the remaining 1/3 amounts of concentrated sulfuric acid with 93% of concentration into a raw material dripping tank B3;
② preheating the reaction kettle 1 to 60 deg.C, starting stirring, opening the valve at the bottom of the raw material dripping tank A2, and slowly dripping ammonium thiocyanate solution into the reaction kettle 1;
③ observing the change of the concentration of sulfuric acid in the reaction kettle 1 through an acidimeter 7, opening a valve at the bottom of the raw material dripping tank B3 when the concentration is reduced to 60%, and dripping concentrated sulfuric acid into the reaction kettle 1;
④, keeping the temperature of the reaction kettle between 60 and 70 ℃ and the pressure between 0 and 0.2MPa by controlling the dropping speed of ammonium thiocyanate, and keeping the acidity of the reaction kettle between 60 and 65 percent by controlling the dropping speed of concentrated sulfuric acid;
⑤ the carbon oxysulfide gas generated by the reaction enters a condenser 4 to remove water vapor and then enters a drier 8 to be dried;
⑥ the dried carbonyl sulfide gas is filled into the product bottle 10 by the compressor 9.
The synthesis reaction was completed after 3 hours to obtain 18.5kg of carbonyl sulfide with a yield of 95% and an analyzed product purity of 97.5%.
Example 2
①, diluting 2/3 of concentrated sulfuric acid with theoretical feeding amount to 65% of concentration, adding the diluted concentrated sulfuric acid into the reaction kettle 1, adding a 65% solution prepared by 25kg of ammonium thiocyanate into a raw material dripping tank A2, and adding the remaining 1/3 amounts of concentrated sulfuric acid with 93% of concentration into a raw material dripping tank B3;
② preheating the reaction kettle 1 to 50 deg.C, stirring, opening the valve at the bottom of the raw material dripping tank A2, and slowly dripping ammonium thiocyanate solution into the reaction kettle 1;
③ observing the change of the concentration of sulfuric acid in the reaction kettle 1 through an acidimeter 7, opening a valve at the bottom of the raw material dripping tank 2 when the concentration is reduced to 55%, and dripping concentrated sulfuric acid into the reaction kettle;
④, keeping the temperature of the reaction kettle between 50 and 60 ℃ and the pressure between 0 and 0.2MPa by controlling the dropping speed of ammonium thiocyanate, and keeping the acidity of the reaction kettle between 55 and 60 percent by controlling the dropping speed of concentrated sulfuric acid;
⑤ the carbon oxysulfide gas generated by the reaction enters a condenser 4 from the outlet to remove water vapor and then enters a dryer 8 for drying;
⑥ the dried carbonyl sulfide gas is filled into the product bottle 10 by the compressor 9.
The synthesis reaction was completed after 3 hours to obtain 18.2kg of carbonyl sulfide with a yield of 93.4% and an analytical product purity of 97.2%.
Claims (2)
1. The utility model provides a device of preparation carbonyl sulfide gas, is formed its characterized in that by reation kettle (1), raw materials dropwise add jar A (2), raw materials dropwise add jar B (3), condenser (4), desicator (8), compressor (9), product bottle (10) meet through the pipeline: reation kettle (1) top meet with raw materials dropwise add jar A (2), raw materials dropwise add jar B (3) respectively through the pipeline, raw materials dropwise add jar A (2), raw materials dropwise add jar B (3) bottom are equipped with the valve, reation kettle (1) on connect thermometer (5), manometer (6) and acidimeter (7) respectively, condenser (4) entry and the exit tube coupling of reation kettle (1), desicator (8) entry and condenser (4) export meet, desicator (8) export meets with compressor (9) entry, compressor (9) export meet with product bottle (10).
2. An apparatus for producing carbonyl sulfide gas as claimed in claim 1, wherein: the dryer (8) is filled with anhydrous calcium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920726269.6U CN210065188U (en) | 2019-05-20 | 2019-05-20 | Device for preparing carbonyl sulfide gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920726269.6U CN210065188U (en) | 2019-05-20 | 2019-05-20 | Device for preparing carbonyl sulfide gas |
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| CN210065188U true CN210065188U (en) | 2020-02-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127702A (en) * | 2019-05-20 | 2019-08-16 | 大连科利德光电子材料有限公司 | Prepare the method and device of carbonyl sulfide gas |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127702A (en) * | 2019-05-20 | 2019-08-16 | 大连科利德光电子材料有限公司 | Prepare the method and device of carbonyl sulfide gas |
| CN110127702B (en) * | 2019-05-20 | 2024-03-19 | 大连科利德光电子材料有限公司 | Method and device for preparing carbonyl sulfide gas |
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