CN109053364A - The manufacturing method of 2 cbloropropane isopropyl chloride - Google Patents
The manufacturing method of 2 cbloropropane isopropyl chloride Download PDFInfo
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- CN109053364A CN109053364A CN201810933957.XA CN201810933957A CN109053364A CN 109053364 A CN109053364 A CN 109053364A CN 201810933957 A CN201810933957 A CN 201810933957A CN 109053364 A CN109053364 A CN 109053364A
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- reaction kettle
- passed
- gas
- cbloropropane isopropyl
- hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses the manufacturing methods of 2 cbloropropane isopropyl chloride, comprising the following steps: after so that the inside of reaction kettle is formed vacuum state, protective gas S1, is passed through into reaction kettle；S2, catalyst and isopropanol are added into the reaction kettle full of protective gas, reaction kettle is heated；S3, hydrogen chloride gas is slowly passed through into reaction kettle；After S4, temperature after being passed through hydrogen chloride gas in reaction kettle top out, stops being passed through for hydrogen chloride gas, obtain 2 cbloropropane isopropyl chloride.The present invention is reacted using gaseous hydrogen chloride, gaseous hydrogen chloride does not have corrosiveness, corrosion will not be generated to reaction kettle, and without oxygen, only inert gas in reaction kettle, and the temperature of reaction kettle is not less than 100 DEG C, so that the water in reaction kettle exists in gaseous form, it ensure that hydrogen chloride exists always in gaseous form, ensure that the stability and safety of production procedure, reduce the generation of production accident.
Description
Technical field
The present invention relates to chemical production technical field more particularly to the manufacturing methods of 2 cbloropropane isopropyl chloride.
Background technique
2 cbloropropane isopropyl chloride, it is not soluble in water, it is dissolved in toluene, methanol, ether, is stable colourless liquid.2 cbloropropane isopropyl chloride is usually
It is synthesized using isopropanol and hydrochloric acid, but the corrosivity of liquid hydrochloric acid is strong, is easy to corrode reaction kettle, so that reaction kettle
Service life reduce, and reactivity is low, and finally obtained finished product is low, so that the production cost increases, and productivity effect
But it cannot improve.
Therefore, we have proposed the manufacturing methods of 2 cbloropropane isopropyl chloride for solving the above problems.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and the manufacturer of the 2- chloropropane proposed
Method.
The manufacturing method of 2 cbloropropane isopropyl chloride, comprising the following steps:
S1, using vacuum pump by reaction kettle air extract out, make reaction kettle inside formed vacuum state after, continue to
Protective gas is passed through in reaction kettle；
S2, catalyst and isopropanol are added into the reaction kettle full of protective gas, reaction kettle is heated, reaction kettle is made
Interior temperature is increased to 100 DEG C -120 DEG C, and keeps temperature-resistant in reaction kettle；
S3, hydrogen chloride gas is slowly passed through into reaction kettle, and by the way that protectiveness gas is passed through or extracted out into reaction kettle
Body, so that the pressure in reaction kettle keeps balance；
S4, the temperature using the temperature change in thermometer measure reaction kettle, after being passed through hydrogen chloride gas in reaction kettle
After topping out, stops being passed through for hydrogen chloride gas, obtain 2 cbloropropane isopropyl chloride.
Preferably, the reaction kettle is made of stainless steel material, and the purity of isopropanol is 100%.
Preferably, the protective gas is nitrogen or argon gas, and reaction kettle stops after pressure reaches 90kPa-150kPa
Only it is passed through protective gas.
Preferably, the catalyst is iron or halogenation spherical alumina, and the purity of iron is 99.99 %, and the diameter of iron is
0.04mm-0.06mm, and the partial size of spherical halogenation aluminium oxide is 3mm-4 mm, and the pore capacity in halogenation spherical alumina is
0.6ml/g-0.8ml/g。
Preferably, it is 90kPa-220 kPa that the pressure in the reaction kettle, which keeps pressure when balance,.
Preferably, the chemical synthesis equation of the 2 cbloropropane isopropyl chloride is
The beneficial effects of the present invention are:
1, of the invention, it is reacted using gaseous hydrogen chloride, gaseous hydrogen chloride does not have corrosiveness, will not be to reaction
Kettle generates corrosion, and without oxygen, only inert gas in reaction kettle, and the temperature of reaction kettle is not less than 100 DEG C, so that
Water in reaction kettle exists in gaseous form, ensure that hydrogen chloride exists always in gaseous form, ensure that production procedure
Stability and safety, reduce the generation of production accident.
2, of the invention, by reacting to each other between gas, and in the presence of a catalyst, improve between reactant
Contact area so that reaction speed accelerate, the conversion rate of reaction is also improved, so that mentioning under identical production cost
The high benefit of production, to improve economic well-being of workers and staff.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment one
The manufacturing method of 2 cbloropropane isopropyl chloride, comprising the following steps:
S1, the air in reaction kettle made of stainless steel material is extracted out using vacuum pump, forms the inside of reaction kettle
After vacuum state, continue to be passed through nitrogen into reaction kettle, so that the pressure in reaction kettle stops being passed through protectiveness after being 120kPa
Gas；
S2, to full of protective gas reaction kettle in be added purity be 99.99%, the iron 10g that diameter is 0.05mm and
The isopropanol 300ml that purity is 100%, reaction kettle is heated, the temperature in reaction kettle is made to be increased to 110 DEG C, and keeps reacting
It is temperature-resistant in kettle；
S3, the hydrogen chloride gas that 310ml is slowly passed through into reaction kettle, and by the way that guarantor is passed through or extracted out into reaction kettle
Shield property gas, so that the pressure in reaction kettle is maintained in 180kPa；
S4, the temperature using the temperature change in thermometer measure reaction kettle, after being passed through hydrogen chloride gas in reaction kettle
After topping out, stop being passed through for hydrogen chloride gas, obtain 2 cbloropropane isopropyl chloride, the chemical synthesis equation of 2 cbloropropane isopropyl chloride is
Embodiment two
The manufacturing method of 2 cbloropropane isopropyl chloride, comprising the following steps:
S1, the air in reaction kettle made of stainless steel material is extracted out using vacuum pump, forms the inside of reaction kettle
After vacuum state, continue to be passed through argon gas into reaction kettle, so that the pressure in reaction kettle stops being passed through protectiveness after being 120kPa
Gas；
S2, to full of protective gas reaction kettle in be added partial size be 3mm, the halogenation ball that pore capacity is 0.7ml/g
The isopropanol 300ml that shape aluminium oxide 10g and purity are 100%, reaction kettle is heated, the temperature in reaction kettle is made to be increased to 120
DEG C, and keep temperature-resistant in reaction kettle；
S3, hydrogen chloride gas 310ml is slowly passed through into reaction kettle, and by the way that protection is passed through or extracted out into reaction kettle
Property gas, so that the pressure in reaction kettle is maintained in 180kPa；
S4, the temperature using the temperature change in thermometer measure reaction kettle, after being passed through hydrogen chloride gas in reaction kettle
After topping out, stop being passed through for hydrogen chloride gas, obtain 2 cbloropropane isopropyl chloride, the chemical synthesis equation of 2 cbloropropane isopropyl chloride is
Comparative example one
Be added into reaction kettle the purity of 10g be 99.99%, the iron that diameter is 0.05mm and the liquid that purity is 100%
Isopropanol 300ml, and the liquid hydrogen chloride of 310ml is added, it is 120 DEG C in temperature, pressure is reacted under conditions of being 180kPa
It is temperature-resistant in reaction kettle.
Comparative example two
Into reaction kettle be added 10g partial size be 3mm, the halogenation spherical alumina and purity that pore capacity is 0.7ml/g
For 100% liquid isopropanol 300ml, and the liquid hydrogen chloride of 310ml is added, is 120 DEG C in temperature, pressure 180kPa
Under conditions of be reacted to it is temperature-resistant in reaction kettle.
2 cbloropropane isopropyl chloride made of embodiment one and embodiment two is analyzed to the residual of hydrogen chloride gas by gas-chromatography
Rate, comparative example one and comparative example two, come the residual rate of analyzing liquid hydrogen chloride, it is as shown in the table to analyze result by liquid chromatogram:
| Embodiment one | Embodiment two | Comparative example one | Comparative example two | |
| Residual rate (%) | 7.2 | 7.3 | 32.6 | 34.2 |
Based on the analysis results it is recognised that in 2 cbloropropane isopropyl chloride made of embodiment one and embodiment two hydrogen chloride gas it is residual
Allowance is few, and the residual quantity of liquid hydrogen chloride is larger in 2 cbloropropane isopropyl chloride made of comparative example one and comparative example two, illustrates the present invention
The production rate of the 2 cbloropropane isopropyl chloride of the manufacturing method of the 2 cbloropropane isopropyl chloride of proposition is high, and reactivity is high, and the pick-up rate of finished product is big.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
- The manufacturing method of 1.2- chloropropane, which comprises the following steps:S1, the air in reaction kettle is extracted out using vacuum pump, after so that the inside of reaction kettle is formed vacuum state, is continued to reaction Protective gas is passed through in kettle；S2, catalyst and isopropanol are added into the reaction kettle full of protective gas, reaction kettle is heated, is made in reaction kettle Temperature is increased to 100 DEG C -120 DEG C, and keeps temperature-resistant in reaction kettle；S3, it is slowly passed through hydrogen chloride gas into reaction kettle, and by the way that protective gas is passed through or extracted out into reaction kettle, makes The pressure obtained in reaction kettle keeps balance；S4, the temperature stopping using the temperature change in thermometer measure reaction kettle, after being passed through hydrogen chloride gas in reaction kettle After raising, stops being passed through for hydrogen chloride gas, obtain 2 cbloropropane isopropyl chloride.
- 2. the manufacturing method of 2 cbloropropane isopropyl chloride according to claim 1, which is characterized in that the reaction kettle is stainless steel material It is made, the purity of isopropanol is 100%.
- 3. the manufacturing method of 2 cbloropropane isopropyl chloride according to claim 1, which is characterized in that the protective gas be nitrogen or Argon gas, and reaction kettle stops being passed through protective gas after pressure reaches 90kPa-150kPa.
- 4. the manufacturing method of 2 cbloropropane isopropyl chloride according to claim 1, which is characterized in that the catalyst is iron or halogenation ball Shape aluminium oxide, and the purity of iron is 99.99%, the diameter of iron are 0.04mm-0.06mm, and the partial size of spherical halogenation aluminium oxide For 3mm-4mm, the pore capacity in halogenation spherical alumina is 0.6ml/g-0.8ml/g.
- 5. the manufacturing method of 2 cbloropropane isopropyl chloride according to claim 1, which is characterized in that the pressure in the reaction kettle is kept Pressure when balance is 90kPa-220kPa.
- 6. the manufacturing method of 2 cbloropropane isopropyl chloride according to claim 1, which is characterized in that the chemical synthesis of the 2 cbloropropane isopropyl chloride Equation is
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1667110A1 (en) * | 1966-04-21 | 1971-11-04 | Ici Ltd | Process for the preparation of an alumina catalyst |
| CN1250496C (en) * | 2001-11-30 | 2006-04-12 | 鹿岛化学株式会社 | Process for producing isopropyl chloride |
| CN1849281A (en) * | 2003-09-08 | 2006-10-18 | 巴斯福股份公司 | Method for producing haloalkanes from alcohols |
| CN105399595A (en) * | 2015-12-30 | 2016-03-16 | 济南诚汇双达化工有限公司 | Preparation method of tert-butyl chloride |
| CN106336341A (en) * | 2016-08-22 | 2017-01-18 | 中南林业科技大学 | Process for synthesizing ethyl chloride |
| CN107814684A (en) * | 2017-10-30 | 2018-03-20 | 安徽东至广信农化有限公司 | A kind of method of gaseous hydrogen chloride synthesis chloromethanes |
-
2018
- 2018-08-16 CN CN201810933957.XA patent/CN109053364A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1667110A1 (en) * | 1966-04-21 | 1971-11-04 | Ici Ltd | Process for the preparation of an alumina catalyst |
| CN1250496C (en) * | 2001-11-30 | 2006-04-12 | 鹿岛化学株式会社 | Process for producing isopropyl chloride |
| CN1849281A (en) * | 2003-09-08 | 2006-10-18 | 巴斯福股份公司 | Method for producing haloalkanes from alcohols |
| CN105399595A (en) * | 2015-12-30 | 2016-03-16 | 济南诚汇双达化工有限公司 | Preparation method of tert-butyl chloride |
| CN106336341A (en) * | 2016-08-22 | 2017-01-18 | 中南林业科技大学 | Process for synthesizing ethyl chloride |
| CN107814684A (en) * | 2017-10-30 | 2018-03-20 | 安徽东至广信农化有限公司 | A kind of method of gaseous hydrogen chloride synthesis chloromethanes |
Non-Patent Citations (1)
| Title |
|---|
| BUKHANKO, NATALIA ETAL.: "Gas phase synthesis of isopropyl chloride from isopropanol and HCl over alumina and flexible 3-D carbon foam supported catalysts", 《APPLIED CATALYSIS A-GENERAL》 * |
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Application publication date: 20181221 |