CN106243147A - Methyl mercaptan tin compound and preparation method thereof - Google Patents
Methyl mercaptan tin compound and preparation method thereof Download PDFInfo
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- CN106243147A CN106243147A CN201610602451.1A CN201610602451A CN106243147A CN 106243147 A CN106243147 A CN 106243147A CN 201610602451 A CN201610602451 A CN 201610602451A CN 106243147 A CN106243147 A CN 106243147A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/22—Tin compounds
- C07F7/226—Compounds with one or more Sn-S linkages
Abstract
The invention discloses the preparation method of a kind of methyl mercaptan tin compound, molecular formula is:
Description
Technical field:
The present invention relates to a kind of methyl mercaptan tin compound and preparation method thereof, more particularly, relate to a kind of PVC thermally-stabilised
Methyl mercaptan tin compound of agent and preparation method thereof.
Background technology:
Organo-tin compound is mainly used in polyvinyl chloride resin as a kind of heat stabilizer, and wherein United States Patent (USP) has many, main
If butyl tin and tin octylate, because propyl group stannum scent of, and ethyl stannum is poisonous and is replaced.
Methyl stannum double isooctyl mercaptoacetate (TM-181) of Morton chemical company of U.S. exploitation is a kind of of many uses
High Efficiency Thermal stabilizer, its Theil indices is 19%-20%, hence it is evident that higher than butyl tin and tin octylate (Theil indices is about 16%), and
There is good intermiscibility with TM-181 with other auxiliary agents, the transparency of product can be improved, owing to wherein there being an a certain proportion of first
Ji Xi, its initial coloring is preferable.
The preparation method of methyl stannum double isooctyl mercaptoacetate is a lot, but technical process is the most more complicated, and cost recovery
High.In order to solve the problems referred to above, Chinese patent application prospectus 94109586X dimethyl sulfone makees catalyst, in temperature
In the range of 150-250 DEG C, reaction pressure is at 6.0-7.0MPa, and the response time is 1-8 hour, reacts generation two by the first step
Methyl dichloro stannum and tin methyltrichloride mixture intermediate；Second step reaction is that raw material midbody is dissolved in TGA
In different monooctyl ester, dripping ammonia, make pH value arrive neutrality, its response time is 1-5 hour, and reaction temperature is 30-80 DEG C.But this system
Preparation Method still needs to synthetic intermediate in a high voltage state, and technological requirement is high, and preparation cost is the highest.Its another shortcoming is
Two step reactions are to carry out in sour environment, easily cause raw material midbody superfluous, and react insufficient.
Summary of the invention
An object of the present invention is to provide a kind of methyl mercaptan tin compound.
The two of the purpose of the present invention are to provide the preparation method of a kind of methyl mercaptan tin compound.
The these and other objects of the present invention will be come to embody further by the following detailed description and explanation.
The methyl mercaptan tin compound of the present invention, its molecular formula is:
The preparation method of the methyl mercaptan tin compound of the present invention, comprises the steps:
A, prepare methyl chloride tin compound intermediate
Adding in chlorinating container by the stannum sheet measured, catalyst, water adds in tourie, and tourie is with absorption kettle even
Connecing, start stirring, be passed through chlorine while stirring, controlling reaction temperature is: 200-300 degree, the response time is 3-6 hour, then
Closing chlorine valve, open monochloro methane valve and start to be passed through, the response time is 4-10 hour, after stannum sheet reacts completely, and chlorine
Terminate when methane no longer reacts；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 150-
280 degree, open falling film absorbing device, under negative pressure state, absorb that i.e. to obtain methyl chloride tin compound intermediate water-soluble 2-6 hour
Liquid；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution that step A is obtained, isooctyl thioglycolate, sodium sulfide, carbonic acid
Hydrogen sodium, catalyst and water adds in synthesis reactor, reacts 1-5 hour, then blowing, layering under room temperature, organic facies is added go from
Sub-water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature:
70-98 degree；Negative pressure: 0.01-0.15MPa；Response time: 2-5 hour, the final products then lower the temperature, filtered.
It is an option that the preparation method of the methyl mercaptan tin compound of the present invention, comprise the steps:
A, prepare methyl chloride tin compound intermediate
Adding in chlorinating container by the stannum sheet measured, catalyst, deionized water adds in tourie, tourie and suction
Receipts still connects, and starts stirring, is passed through chlorine while stirring, controls reaction temperature and is: 200-300 degree, the response time is that 4-5 is little
Time, it being then shut off chlorine valve, open monochloro methane valve and start to be passed through, the response time is 6-8 hour, treats that stannum sheet reacts completely
After, terminate when chloromethanes no longer reacts；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature
190-240 degree, opens falling film absorbing device, absorbs 3-5 hour and i.e. obtain methyl chloride tin compound intermediate under negative pressure state
Aqueous solution；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution that step A is obtained, isooctyl thioglycolate, sodium sulfide, carbonic acid
Hydrogen sodium, catalyst and water adds in synthesis reactor, reacts 1-5 hour, then blowing, layering under room temperature, organic facies is added go from
Sub-water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature:
80-95 degree；Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered.
It is preferred that the preparation method of the methyl mercaptan tin compound of the present invention, comprise the steps: A, prepare methyl chloride
Change tin compound intermediate
The catalyst of the stannum sheet of 100-200 kilogram and 3-8 kilogram is added in chlorinating container, 150-300 kilogram go from
Sub-water adds in tourie, and tourie is connected with absorption kettle, starts stirring, is passed through the chlorine of 50-130 kilogram while stirring, control
Reaction temperature processed is: 200-300 degree, and the response time is 4-5 hour, is then shut off chlorine valve, opens monochloro methane valve and opens
Beginning is passed through, and the response time is 6-8 hour, after stannum sheet reacts completely, terminates when monochloro methane no longer reacts, adding of monochloro methane
Enter amount and be 30-80 kilogram；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 190-240
Degree, opens falling film absorbing device, absorbs 3-5 hour and i.e. obtain methyl chloride tin compound intermediate water solution under negative pressure state,
Yield is 98.5%；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution of 150-250 kilogram that step A is obtained, the mercapto of 80-120 kilogram
The different monooctyl ester of guanidine-acetic acid, the sodium sulfide of 20-50 kilogram, the sodium bicarbonate of 30-60 kilogram, 0.2-0.8 kg catalyst and 150-250
Kilogram deionized water add in synthesis reactor, react 1-5 hour under room temperature, then blowing, layering, organic facies added 200 public
Jin deionized water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is:
Temperature: 80-95 degree；Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered, yield is
98.0%.
The preparation method of the methyl mercaptan tin compound of the present invention, comprises the steps:
A, prepare methyl chloride tin compound intermediate
The catalyst of the stannum sheet of 120-160 kilogram and 4-7 kilogram is added in chlorinating container, 180-250 kilogram go from
Sub-water adds in tourie, and tourie is connected with absorption kettle, starts stirring, is passed through the chlorine of 80-110 kilogram while stirring, control
Reaction temperature processed is: 200-300 degree, and the response time is 4-5 hour, is then shut off chlorine valve, opens monochloro methane valve and opens
Beginning is passed through, and the response time is 6-8 hour, after stannum sheet reacts completely, terminates when monochloro methane no longer reacts, adding of monochloro methane
Enter amount and be 50-70 kilogram；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 190-240
Degree, opens falling film absorbing device, absorbs 3-5 hour and i.e. obtain methyl chloride tin compound intermediate water solution under negative pressure state,
Yield is 98.5%；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution of 180-210 kilogram that step A is obtained, the mercapto of 90-110 kilogram
The different monooctyl ester of guanidine-acetic acid, the sodium sulfide of 30-40 kilogram, the sodium bicarbonate of 30-50 kilogram, 0.3-0.6 kg catalyst and 180-220
Kilogram deionized water add in synthesis reactor, react 1-5 hour under room temperature, then blowing, layering, organic facies added 200 public
Jin deionized water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is:
Temperature: 80-95 degree；Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered, yield is
98.0%.
In the preparation method of the methyl mercaptan tin compound of the present invention, described catalyst be monomethyl ammonium chloride, two
Ammonio methacrylate, trimethyl ammonium chloride or tetramethyl ammonium chloride, 213 ion exchange resins.
In the preparation method of the methyl mercaptan tin compound of the present invention, the design pressure of described chlorinating container is:
2.4MPa, operating pressure is: 1.6MPa, diameter: DN1100, cylinder height: 4200mm, inside has chloromethanes conduit 3900mm, stirs
Mixing speed is 470 revs/min, and mirror mouth, thermometer mouth, gauge port are observed in sampling.
In the preparation method of the methyl mercaptan tin compound of the present invention, described Methyl stannum mercaptide compound molecule formula
For:
It is prepared as follows, comprises the steps:
A. the preparation of methyl chloride tin compound intermediate
By the stannum sheet of 140 kilograms, the specification of stannum sheet is: 100mmx150mmx35mm, 6 kilograms of tetramethyl ammonium chloride ammonium salts
Catalyst adds in chlorinating container, and 200 kilograms of deionized waters add in tourie, and tourie is connected with absorption kettle, this chlorination
The design pressure of reactor is: 2.4MPa, and operating pressure is: 1.6MPa, diameter: DN1100, and cylinder height: 4200mm inside has
Chloromethanes conduit 3900mm, mixing speed is 470 revs/min, has sampling and observes mirror mouth, thermometer mouth and gauge port, opens
Dynamic stirring, is passed through 90 kilograms of chlorine while stirring, and controlling reaction temperature is 260 degree, and the response time is 4 hours；It is then shut off chlorine
Air valve, opens monochloro methane valve and starts to be passed through, and the response time is 6 hours, and the addition of monochloro methane is 64 kilograms；Treat stannum
After sheet reacts completely, terminate when chloromethanes no longer reacts；Open chlorination tank and absorption kettle connects valve, material is imported absorption kettle
In, keep temperature 240 degree, open falling film absorbing device, absorb under negative pressure state and i.e. obtain in methyl chloride tin compound for 5 hours
Mesosome aqueous solution 498kg.Yield is 98.5%；
B, the preparation of methyl mercaptan tin compound
By 200 kilograms, the methyl chloride tin compound intermediate water solution of content 119.6 kilograms, the sulfydryl second of 102 kilograms
The different monooctyl ester of acid, the sodium sulfide of 39 kilograms, the sodium bicarbonate of 42 kilograms, catalyst and 200 kilograms of deionized waters add in synthesis reactor,
React 1-5 hour under room temperature, then blowing, layering, organic facies is added 200 kilograms of deionized waters stir 30 minutes static, point
Layer；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature is 80 degree, and negative pressure is-0.098MPa,
Response time is 3.0 hours, and the final products methyl mercaptan tin compound 180kg then lower the temperature, filtered, yield is 98.0%.
Reaction equation is as follows:
The preparation method of the methyl mercaptan tin compound that the present invention provides, have employed monomethyl chloride former as reaction
Material, it is more excellent than the stability of dimethyl chloride, creates sulphur bridge, adds sulfur stannum key, increases molecular weight, every
Performance is better than existing methyl tin heat stabilizer, can be as a kind of novel, more preferable PVC heat stabilizer of effect.And method
Technique is simple, and mild condition is easy and simple to handle, is easily controlled, the features such as raw material is easily purchased, safe and reliable, before having good application
Scape.
Methyl mercaptan tin compound and preparation method thereof
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
In the present invention, refering in particular to as non-, all of amount, part are unit of weight, and all of raw material all can be from market
Buy.
Detailed description of the invention
Embodiment 1: Methyl stannum mercaptide compound molecule formula is:
It is prepared as follows, comprises the steps:
A. the preparation of methyl chloride tin compound intermediate
By the stannum sheets of 140 kilograms (content is: 99.99%, technical grade), the specification of stannum sheet is: 100mmx150mmx35mm,
6 kilograms of tetramethyl ammonium chloride ammonium salts catalyst add in chlorinating container, and 200 kilograms of deionized waters add in tourie, inhale
Closed cans is connected with absorption kettle, and the design pressure of this chlorinating container is: 2.4MPa, and operating pressure is: 1.6MPa, diameter:
DN1100, cylinder height: 4200mm, inside have chloromethanes conduit 3900mm, and mixing speed is 470 revs/min, has sampling observation and regards
Jing Kou, thermometer mouth and gauge port etc., start stirring, be passed through 90 kilograms of chlorine (99.9%, technical grade) while stirring, control
Reaction temperature is 260 degree, and the response time is 4 hours；It is then shut off chlorine valve, opens monochloro methane valve and start to be passed through, instead
Being 6 hours between Ying Shi, the addition of monochloro methane is 64 kilograms (content 99.0%, technical grades)；After stannum sheet reacts completely, chlorine
Terminate when methane no longer reacts；Open chlorination tank and absorption kettle connect valve, material is imported in absorption kettle, keep temperature 240 degree,
Open falling film absorbing device, absorb under negative pressure state and within 5 hours, i.e. obtain methyl chloride tin compound intermediate water solution 498kg.
Yield is 98.5%；
B, the preparation of methyl mercaptan tin compound
By 200 kilograms, the methyl chloride tin compound intermediate water solution of content 119.6 kilograms, the sulfydryl second of 102 kilograms
The different monooctyl ester of acid (content is: 99.0%, technical grade), the sodium sulfide (content is: 99.0%, technical grade) of 39 kilograms, 42 kilograms
Sodium bicarbonate (content is: 99.0%, technical grade), the catalyst (213 ion exchange resin) of 0.4 kilogram and 200 kilograms of deionized waters
Add in synthesis reactor, react 1-5 hour under room temperature, then blowing, layering, organic facies is added 200 kilograms of deionized water stirrings
Static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature is 80 degree, negative pressure
For-0.098MPa, the response time is 3.0 hours, the final products methyl mercaptan tin compound 180kg then lower the temperature, filtered, and receives
Rate is 98.0%.
Reaction equation is as follows:
Embodiment 2: Methyl stannum mercaptide compound molecule formula is:
It is prepared as follows, comprises the steps:
A. the preparation of methyl chloride tin compound intermediate
By the stannum sheets of 110 kilograms (content is: 99.99%, technical grade), the specification of stannum sheet is: 100mmx150mmx35mm,
3.5 kilograms of tetramethyl ammonium chloride catalyst add in chlorinating container, and 150 kilograms of deionized waters add in tourie, tourie
Being connected with absorption kettle, the design pressure of this chlorinating container is: 2.4MPa, and operating pressure is: 1.6MPa, diameter: DN1100, cylinder
Height: 4200mm, inside has chloromethanes conduit 3900mm, and mixing speed is 470 revs/min, has sampling and observes mirror mouth, temperature
Meter mouth and gauge port etc., start stirring, is passed through 55 kilograms of chlorine (99.9%, technical grade) while stirring, controls reaction temperature
Being 230 degree, the response time is 4 hours；Being then shut off chlorine valve, open monochloro methane valve and start to be passed through, the response time is 6
Hour, the addition of monochloro methane is 34 kilograms (content 99.0%, technical grades)；After stannum sheet reacts completely, chloromethanes is no longer
Terminate during reaction；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 200 degree, open falling liquid film and inhale
Receiving apparatus, absorbs under negative pressure state and within 4 hours, i.e. obtains methyl chloride tin compound intermediate water solution 408kg.Yield is
96.5%；
B, the preparation of methyl mercaptan tin compound
By 160 kilograms, content is the methyl chloride tin compound intermediate water solution of 89.6 kilograms, the sulfydryl second of 80 kilograms
The different monooctyl ester of acid (content is: 99.0%, technical grade), the sodium sulfide (content is: 99.0%, technical grade) of 25 kilograms, 32 kilograms
Sodium bicarbonate (content is: 99.0%, technical grade), the catalyst (213 ion exchange resin) of 0.3 kilogram and 160 kilograms of deionized waters
Add in synthesis reactor, react 2.5 hours under room temperature, then blowing, layering, organic facies is added 150 kilograms of deionized water stirrings
Static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature is 80 degree, negative pressure
For-0.098MPa, the response time is 3.0 hours, the final products methyl mercaptan tin compound 180kg then lower the temperature, filtered, and receives
Rate is 98.0%.
Reaction equation is as follows:
Embodiment 3: Methyl stannum mercaptide compound molecule formula is:
It is prepared as follows, comprises the steps:
A. the preparation of methyl chloride tin compound intermediate
By the stannum sheets of 180 kilograms (content is: 99.99%, technical grade), the specification of stannum sheet is: 100mmx150mmx35mm,
7.5 kilograms of trimethyl ammonium chloride catalyst add in chlorinating container, and 300 kilograms of deionized waters add in tourie, tourie
Being connected with absorption kettle, the design pressure of this chlorinating container is: 2.4MPa, and operating pressure is: 1.6MPa, diameter: DN1100, cylinder
Height: 4200mm, inside has chloromethanes conduit 3900mm, and mixing speed is 470 revs/min, has sampling and observes mirror mouth, temperature
Meter mouth and gauge port etc., start stirring, is passed through 120 kg chlorine (99.9%, technical grade) while stirring, controls reaction temperature
Being 280 degree, the response time is 5 hours；Being then shut off chlorine valve, open monochloro methane valve and start to be passed through, the response time is
7.5 hours, the addition of monochloro methane was 75 kilograms (content 99.0%, technical grades)；After stannum sheet reacts completely, chloromethanes is not
Terminate when reacting again；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 220 degree, open falling liquid film
Absorption plant, absorbs under negative pressure state and within 5 hours, i.e. obtains methyl chloride tin compound intermediate water solution 548kg.Yield is
93.5%；
B, the preparation of methyl mercaptan tin compound
By 250 kilograms, content is the methyl chloride tin compound intermediate water solution of 169.8 kilograms, the sulfydryl of 110 kilograms
2-ethyl hexyl ethanoate (content is: 99.0%, technical grade), the sodium sulfide (content is: 99.0%, technical grade) of 45 kilograms, 55 kilograms
Sodium bicarbonate (content is: 99.0%, technical grade), the catalyst (213 ion exchange resin) of 0.8 kilogram and 250 kilograms of deionizations
Water adds in synthesis reactor, reacts 4.5 hours, then blowing, layering under room temperature, is stirred by organic facies 250 kilograms of deionized waters of addition
Mix static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature is 90 degree, negative
Pressure is-0.098MPa, and the response time is 4.0 hours, the final products methyl mercaptan tin compound 245kg then lower the temperature, filtered,
Yield is 95.0%.
Reaction equation is as follows:
Claims (8)
1. a methyl mercaptan tin compound, it is characterised in that molecular formula is:
。
The preparation method of methyl mercaptan tin compound the most according to claim 1, it is characterised in that comprise the steps:
A, prepare methyl chloride tin compound intermediate
Adding in chlorinating container by the stannum sheet measured, catalyst, water adds in tourie, and tourie is connected with absorption kettle,
Starting stirring, be passed through chlorine while stirring, controlling reaction temperature is: 200-300 degree, the response time is 3-6 hour, is then shut off
Chlorine valve, opens monochloro methane valve and starts to be passed through, and the response time is 4-10 hour, after stannum sheet reacts completely, and chloromethanes
No longer terminate during reaction；Open chlorination tank and absorption kettle connect valve, material is imported in absorption kettle, keep temperature 150-280 degree,
Open falling film absorbing device, absorb under negative pressure state 2-6 hour and i.e. obtain methyl chloride tin compound intermediate water solution；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution that step A is obtained, isooctyl thioglycolate, sodium sulfide, sodium bicarbonate,
Catalyst and water add in synthesis reactor, react 1-5 hour, then blowing, layering, organic facies is added deionized water and stirs under room temperature
Mix static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature: 70-98 degree；
Negative pressure: 0.01-0.15MPa；Response time: 2-5 hour, the final products then lower the temperature, filtered.
The preparation method of methyl mercaptan tin compound the most according to claim 2, it is characterised in that comprise the steps:
A, prepare methyl chloride tin compound intermediate
Adding in chlorinating container by the stannum sheet measured, catalyst, water adds in tourie, and tourie is connected with absorption kettle,
Starting stirring, be passed through chlorine while stirring, controlling reaction temperature is: 200-300 degree, the response time is 4-5 hour, is then shut off
Chlorine valve, opens monochloro methane valve and starts to be passed through, and the response time is 6-8 hour, and after stannum sheet reacts completely, chloromethanes is not
Terminate when reacting again；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, keep temperature 190-240 degree, open
Falling film absorbing device, absorbs under negative pressure state 3-5 hour and i.e. obtains methyl chloride tin compound intermediate water solution；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution that step A is obtained, isooctyl thioglycolate, sodium sulfide, sodium bicarbonate,
Catalyst and water add in synthesis reactor, react 1-5 hour, then blowing, layering, organic facies is added deionized water and stirs under room temperature
Mix static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature: 80-95 degree；
Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered.
The preparation method of methyl mercaptan tin compound the most according to claim 2, it is characterised in that comprise the steps:
A, prepare methyl chloride tin compound intermediate
The catalyst of the stannum sheet of 100-200 kilogram and 3-8 kilogram is added in chlorinating container, the deionization of 150-300 kilogram
Water adds in tourie, and tourie is connected with absorption kettle, starts stirring, is passed through the chlorine of 50-130 kilogram while stirring, controls
Reaction temperature is: 200-300 degree, and the response time is 4-5 hour, is then shut off chlorine valve, opens monochloro methane valve and starts
Being passed through, the response time is 6-8 hour, after stannum sheet reacts completely, terminates when monochloro methane no longer reacts, the addition of monochloro methane
Amount is for 30-80 kilogram；Open chlorination tank and absorption kettle connect valve, material is imported in absorption kettle, keep temperature 190-240 degree,
Open falling film absorbing device, absorb under negative pressure state 3-5 hour and i.e. obtain methyl chloride tin compound intermediate water solution, yield
It is 98.5%；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution of 150-250 kilogram that step A is obtained, the sulfydryl second of 80-120 kilogram
The different monooctyl ester of acid, the sodium sulfide of 20-50 kilogram, the sodium bicarbonate of 30-60 kilogram, 0.2-0.8 kg catalyst and 150-250 kilogram
Deionized water add in synthesis reactor, react 1-5 hour under room temperature, then blowing, layering, organic facies addition 200 kilograms gone
Ionized water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature:
80-95 degree；Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered, yield is
98.0%.
The preparation method of methyl mercaptan tin compound the most according to claim 2, it is characterised in that comprise the steps:
A, prepare methyl chloride tin compound intermediate
The catalyst of the stannum sheet of 120-160 kilogram and 4-7 kilogram is added in chlorinating container, the deionization of 180-250 kilogram
Water adds in tourie, and tourie is connected with absorption kettle, starts stirring, is passed through the chlorine of 80-110 kilogram while stirring, controls
Reaction temperature is: 200-300 degree, and the response time is 4-5 hour, is then shut off chlorine valve, opens monochloro methane valve and starts
Being passed through, the response time is 6-8 hour, after stannum sheet reacts completely, terminates when monochloro methane no longer reacts, the addition of monochloro methane
Amount is for 50-70 kilogram；Open chlorination tank and absorption kettle connect valve, material is imported in absorption kettle, keep temperature 190-240 degree,
Open falling film absorbing device, absorb under negative pressure state 3-5 hour and i.e. obtain methyl chloride tin compound intermediate water solution, yield
It is 98.5%；
B, the preparation of methyl mercaptan tin compound
The methyl chloride tin compound intermediate water solution of 180-210 kilogram that step A is obtained, the sulfydryl second of 90-110 kilogram
The different monooctyl ester of acid, the sodium sulfide of 30-40 kilogram, the sodium bicarbonate of 30-50 kilogram, 0.3-0.6 kg catalyst and 180-220 kilogram
Deionized water add in synthesis reactor, react 1-5 hour under room temperature, then blowing, layering, organic facies addition 200 kilograms gone
Ionized water stirs static, layering in 30 minutes；Organic facies carries out decompression distillation again, and what decompression was distilled control condition is: temperature:
80-95 degree；Negative pressure: 0.05-0.1MPa；Response time: 3-4 hour, the final products then lower the temperature, filtered, yield is
98.0%.
6. according to the preparation method of the methyl mercaptan tin compound described in claim 2-5, it is characterised in that described catalyst
For monomethyl ammonium chloride, alkyl dimethyl ammonium chloride, trimethyl ammonium chloride or tetramethyl ammonium chloride, 213 ion exchange resins.
7. according to the preparation method of the methyl mercaptan tin compound described in claim 2-5, it is characterised in that preparing methyl chloride
Changing in tin compound intermediate Part, the design pressure of described chlorinating container is: 2.4MPa, and operating pressure is: 1.6MPa,
Diameter: DN1100, cylinder height: 4200mm, inside have chloromethanes conduit 3900mm, and mixing speed is 470 revs/min, and sampling is observed
Mirror mouth, thermometer mouth, gauge port.
8. the preparation method of a methyl mercaptan tin compound, it is characterised in that described Methyl stannum mercaptide compound molecule formula
For:
It is prepared as follows, comprises the steps:
A. the preparation of methyl chloride tin compound intermediate
By the stannum sheet of 140 kilograms, the specification of stannum sheet is: 100mmx150mmx35mm, 6 kilograms of tetramethyl ammonium chloride ammonium salts catalysis
Agent adds in chlorinating container, and 200 kilograms of deionized waters add in tourie, and tourie is connected with absorption kettle, this chlorination reaction
The design pressure of still is: 2.4MPa, and operating pressure is: 1.6MPa, diameter: DN1100, and cylinder height: 4200mm inside has chloromethane
Alkane conduit 3900mm, mixing speed is 470 revs/min, has sampling and observes mirror mouth, thermometer mouth and gauge port, starts and stir
Mixing, be passed through 90 kilograms of chlorine while stirring, controlling reaction temperature is 260 degree, and the response time is 4 hours；It is then shut off chlorine valve
Door, opens monochloro methane valve and starts to be passed through, and the response time is 6 hours, and the addition of monochloro methane is 64 kilograms；Treat that stannum sheet is complete
After full response, terminate when chloromethanes no longer reacts；Open chlorination tank and absorption kettle connects valve, material is imported in absorption kettle, protect
Hold temperature 240 degree, open falling film absorbing device, absorb under negative pressure state and within 5 hours, i.e. obtain methyl chloride tin compound intermediate
Aqueous solution 498kg.Yield is 98.5%；
B, the preparation of methyl mercaptan tin compound
By 200 kilograms, the methyl chloride tin compound intermediate water solution of content 119.6 kilograms, the TGA of 102 kilograms is different
Monooctyl ester, the sodium sulfide of 39 kilograms, the sodium bicarbonate of 42 kilograms, catalyst and 200 kilograms of deionized waters add in synthesis reactor, room temperature
Lower reaction 1-5 hour, then blowing, layering, organic facies is added 200 kilograms of deionized waters and stirs static, layering in 30 minutes；Again
Organic facies carries out decompression distillation, and what decompression was distilled control condition is: temperature is 80 degree, and negative pressure is-0.098MPa, during reaction
Between be 3.0 hours, the final products methyl mercaptan tin compound 180kg then lower the temperature, filtered, yield is 98.0%.
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