CN105921079B - A method of the polysiloxane oligomers cracking containing chain fluoroalkyl - Google Patents
A method of the polysiloxane oligomers cracking containing chain fluoroalkyl Download PDFInfo
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- CN105921079B CN105921079B CN201610300207.XA CN201610300207A CN105921079B CN 105921079 B CN105921079 B CN 105921079B CN 201610300207 A CN201610300207 A CN 201610300207A CN 105921079 B CN105921079 B CN 105921079B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
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Abstract
The invention discloses a kind of polysiloxane oligomers cracker and cleavage method containing chain fluoroalkyl.The inventive system comprises cracking reaction kettle, insertion tube, condenser pipes, it is characterized by: being equipped with blender in the cracking reaction kettle, one end of insertion tube is inserted into cracking reaction kettle by insert port and is connected to gas distributor, the other end is connected to by pipeline with inert gas tank, one end of condenser pipe is connected by vacuum pipe with vacuum pump, the upper end that the other end receives container and rectifying column with product respectively is connected, and the lower end of rectifying column is connected to by gas phase mouth with cracking reaction kettle.The step of cleavage method: (1) oligomer, catalyst, octadecyl alcolol are added in reaction kettle, stir, vacuumizes, gradually temperature raising, steams front-end volatiles；(2) after isolating front-end volatiles, it is passed through inert gas into reaction kettle, keeps vacuum degree more than -0.9MPa, and gradually temperature raising extraction cracking product.Present invention is mainly used for the polysiloxane oligomers cracking containing chain fluoroalkyl.
Description
Technical field
The present invention relates to a kind of cracker and cleavage methods, and in particular to a kind of polysiloxanes containing chain fluoroalkyl is low
Polymers cracker and cleavage method.
Background technique
Since fluorinated polysiloxane has low surface tension, nonflammable and grease proofing characteristic, it is widely used in defoaming
The multiple fields such as agent, remover, anti-graffiti coatings.But common fluorinated polysiloxane (such as poly- (3,3,3- trifluoro propyl first
Radical siloxane)) it is short due to containing fluorine chain, it is also difficult to achieve the effect that in terms of grease proofing of great satisfaction.It is known that
With the growth containing fluorine chain, the above-mentioned performance of fluorinated polysiloxane macromolecule polyalcohol can further improve.
The ring-opening polymerisation of siloxanes ring body compound is to prepare the important method of polysiloxanes macromolecule polyalcohol, in order to make
It is standby (to refer to that n is the C of 3 and the above integer in this patent containing chain fluoroalkylnF2n+1Polysiloxanes macromolecular group, similarly hereinafter) is poly-
It closes object and needs to obtain corresponding ring body raw material first.Chain fluoroalkyl alkene (RFCH=CH2Or RF-CH2CH=CH2Deng RFFor length
Chain fluoroalkyl) and allyl chloride through Si―H addition reaction chain fluoroalkyl ethyl or chain fluoroalkyl hydroxypropyl methyl dichloro silicon is made
Alkane, product hydrolysis obtain oligomer, and oligomer is reacted using Pintsch process and rectification under vacuum obtains corresponding ring body
Close object.Document Yungk.Kim.J.Org.Chem., 1973, Vol.58 (No.8): 1615-1616, document Yutaka
Furukawa.Journal of Applied Polymer Science, 2001, vol.82,3333-334 and document
A.E.Shamaev.Russian Chemical Bulletin,International Edition,2005,vol.53
(No.10): 2229-2232 reports the above method.
However, since above-mentioned ring body compound boiling point is high, is not easy to steam, or even also steam under the conditions of condition of high vacuum degree slow
Slowly；In addition, polymer viscosity is higher, cause mass-and heat-transfer slow；These reasons cause the distillation process duration often longer,
Production efficiency is low.On the other hand, the alkali catalyst being added in cracking process will lead to fluoroalkyl during Pintsch process
Fluorine atom is removed, and may further generate crosslinking, reduces product yield.
Summary of the invention
The purpose of the present invention is provide a kind of polysiloxane oligomers containing chain fluoroalkyl for prior art problem to split
Solve device, and the method that the cracking of the polysiloxane oligomers containing chain fluoroalkyl is carried out using the cracker.Of the invention
Cleavage method mass-and heat-transfer is effect improved, and inert gas traction makes the ring body product of the generation of cracking be easy to steam, so as to shorten
Distillation process improves production efficiency；In addition, cleavage method of the invention can also prevent the removing of fluorine atom.
To achieve the goals above, present invention employs the following technical solutions:
A kind of polysiloxane oligomers cracker containing chain fluoroalkyl, including cracking reaction kettle, insertion tube, condensation
Pipe, it is characterised in that: blender 12 is equipped in the cracking reaction kettle 5, one end of insertion tube 3 passes through the insertion cracking of insert port 11
It is connected in reaction kettle and with gas distributor 4, the other end is connected to by pipeline 2 with inert gas tank 1, and one end of condenser pipe 7 is logical
It crosses vacuum pipe 10 to be connected with vacuum pump 9, the upper end that the other end receives container 8 and rectifying column 6 with product respectively is connected, rectifying column
Lower end be connected to cracking reaction kettle 5 by gas phase mouth 13.
The gas distributor 4 and the vertical range of 5 bottom of cracking reaction kettle are at least 0.5cm.
The cracking reaction kettle 5 is the cracking container that the thermally conductive flow of oil of high-temperature medium is marked in jacket type and collet.
A method of the cracking of the polysiloxane oligomers containing chain fluoroalkyl, feature are carried out with claim 1 device
It is following steps:
(1) polysiloxane oligomers containing chain fluoroalkyl, catalyst, octadecyl alcolol are added in cracking reaction kettle, are opened
Stirring, starts simultaneously at and vacuumizes, and steps up cracking container contents temperature, steams front-end volatiles；
(2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking reaction kettle, while keeping cracking reaction
Vacuum degree in kettle continues to step up cracking reaction material temperature in kettle extraction cracking product more than -0.9MPa, until
No product continues to produce.
The catalyst is the 0.05~1% of oligomer quality dosage, and the octadecyl alcolol is the 1~5% of oligomer dosage.
The polysiloxane oligomers containing chain fluoroalkyl can use formulaIt indicates, wherein x, y are the integer more than or equal to 4, RFIndicate long-chain
Fluoroalkyl, Me indicate methyl.
The chain fluoroalkyl RFFormula C can be usednF2n+1(CH2)mIt indicates, the integer that wherein n is 3~8, m is 2 or 3.
The R containing chain fluoroalkylFSelected from CF3CF2CF2CF2CH2CH2、CF3CF2CF2CF2CF2CF2CH2CH2、
CF3CF2CF2C(CF3)2CH2CH2CH2One of.
The catalyst is selected from potassium hydroxide, sodium hydroxide, cesium hydroxide, tetramethylammonium hydroxide, potassium carbonate, carbonic acid
One of sodium, calcium carbonate alkaline compound.
As a kind of way of realization, the cracking container have collet, by the fluid in collet to cracking container into
Row heating.
As another way of realization, the cracking container is heated by oil bath or heating mantle etc..
Polysiloxane oligomers cracker containing chain fluoroalkyl of the invention is provided with inert gas supply equipment, lazy
Property gas pipeline and insertion tube, insertion tube connect by inert gas duct with inert gas supply equipment；Insertion tube is by splitting
It solves in container insert port insertion cracking container, and is connected with gas distributor, gas distributor hangs down with cracking container bottom
Straight distance is in 0.5cm or more, but gas distributor should be located at cracking container lower half.Above-mentioned apparatus can introduce inert gas into
It cracks inside the polysiloxane oligomers containing chain fluoroalkyl in container, the sufficiently high vacuum item more than holding -0.9MPa
Under part, then by the draw of inert gas, the ring body product for cracking generation is easier to steam.But it is difficult to when vacuum degree is relatively low
Reach ideal effect.
When carrying out the cracking of the polysiloxane oligomers containing chain fluoroalkyl using above-mentioned apparatus, it should be added in oligomer
Catalyst and octadecyl alcolol.Catalyst can promote to react and develop towards the direction of cyclisation product, and the catalyst is selected from hydroxide
The alkali compounds such as potassium, sodium hydroxide, cesium hydroxide, tetramethylammonium hydroxide, potassium carbonate, sodium carbonate, calcium carbonate, wherein it is preferred that
For potassium hydroxide.The additional amount of catalyst should be controlled 0.05~1%, too low, be difficult to play catalytic action, it is excessively high may
The removing for accelerating fluorine atom on fluoroalkyl, leads to the generation of side reaction.Octadecyl alcolol can improve the poly- of high viscosity chain fluoroalkyl
The mass-and heat-transfer effect of siloxane oligomer, conducive to steaming for the cyclisation product generated is cracked.In addition, octadecyl alcolol can also and alkali
Property catalyst interaction, prevent basic species from may cause the generation of the elimination reaction of fluorine atom and fluorine atom on fluoroalkyl
The crosslinking of further occurrence after removing, to improve the yield of cyclisation product.
Polysiloxane oligomers containing chain fluoroalkyl are prepared using the prior art or literature method: 1) being prepared first containing double
Key fluoroalkyle compound can use CnF2n+1X and Addition on ethylene generate CnF2n+1CH2CH2X, after through removing HX reaction generate
CnF2n+1CH=CH2, n is 4 or 6 in the above formulas, and X is Br or I；Or reacted with hexafluoropropylene dimmer with KF and allyl bromide, bromoallylene,
Generate CF3CF2CF2C(CF3)2CH2CH2CH2.2) fluorine is generated with fluoroalkyle compound containing double bond and allyl chloride Si―H addition reaction
Alkyl methyl dichlorosilane (RFSiMeCl2).3) fluoroalkyl dimethyl dichlorosilane (DMCS) hydrolysis obtains the poly- silicon oxygen containing chain fluoroalkyl
Alkane oligomer.
The present invention by adopting the above-described technical solution, the beneficial effect is that:
1) cleavage method of the invention improves mass-and heat-transfer effect；
2) cleavage method of the invention makes the ring body product of the generation cracked be easy to steam by the traction of inert gas；
3) cleavage method distillation process of the invention shortens, improves production efficiency；
4) cleavage method of the invention can also prevent the removing of fluorine atom.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the polysiloxane oligomers cracker of the invention containing chain fluoroalkyl.
In figure: 1- inert gas tank, 2- pipeline, 3- insertion tube, 4- gas distributor, 5- cracking reaction kettle, 6- rectifying column,
7- condenser pipe, 8- product receive container, 9- vacuum pump, 10- vacuum pipe, 11- insert port, 12- blender, 13- gas phase mouth.
Specific embodiment
The present invention and its specific embodiment are described in further detail below in conjunction with drawings and examples.
Referring to Fig. 1, the present invention includes cracking reaction kettle, insertion tube, condenser pipe, it is characterised in that: the cracking reaction kettle 5
Interior to be equipped with blender 12, one end of insertion tube 3 is inserted into cracking reaction kettle by insert port 11 and is connected to gas distributor 4,
The other end is connected to by pipeline 2 with inert gas tank 1, and one end of condenser pipe 7 is connected by vacuum pipe 10 with vacuum pump 9, separately
The upper end that one end receives container 8 and rectifying column 6 with product respectively is connected, and the lower end of rectifying column passes through gas phase mouth 13 and cracking reaction
Kettle 5 is connected to.
The gas distributor 4 and the vertical range of 5 bottom of cracking reaction kettle are at least 0.5cm.
The cracking reaction kettle 5 is the cracking container that the thermally conductive flow of oil of high-temperature medium is marked in jacket type and collet.
A method of the cracking of the polysiloxane oligomers containing chain fluoroalkyl, feature are carried out with claim 1 device
It is following steps:
(1) polysiloxane oligomers containing chain fluoroalkyl, catalyst, octadecyl alcolol are added in cracking reaction kettle, are opened
Stirring, starts simultaneously at and vacuumizes, and steps up cracking container contents temperature, steams front-end volatiles；
(2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking reaction kettle, while keeping cracking reaction
Vacuum degree in kettle continues to step up cracking reaction material temperature in kettle extraction cracking product more than -0.9MPa, until
No product continues to produce.
The catalyst is the 0.05~1% of oligomer quality dosage, and the octadecyl alcolol is the 1~5% of oligomer dosage.
The polysiloxane oligomers containing chain fluoroalkyl can use formulaIt indicates, wherein x, y are the integer more than or equal to 4, RFIndicate long-chain
Fluoroalkyl, Me indicate methyl.
The chain fluoroalkyl RFFormula C can be usednF2n+1(CH2)mIt indicates, the integer that wherein n is 3~8, m is 2 or 3.
The R containing chain fluoroalkylFSelected from CF3CF2CF2CF2CH2CH2、CF3CF2CF2CF2CF2CF2CH2CH2、
CF3CF2CF2C(CF3)2CH2CH2CH2One of.
The catalyst is selected from potassium hydroxide, sodium hydroxide, cesium hydroxide, tetramethylammonium hydroxide, potassium carbonate, carbonic acid
One of sodium, calcium carbonate alkaline compound.
An example of the present invention is given below
Embodiment 1
1) by RFFor CF3CF2CF2CF2CH2CH21000 mass parts of polysiloxane oligomers containing chain fluoroalkyl, hydrogen-oxygen
Change 5 mass parts of potassium, 20 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and step up and split
Container contents temperature is solved, front-end volatiles are steamed；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.95MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time (present invention in the rectifying time refer to isolate front-end volatiles after start to no product continue extraction when end passed through
The time gone through) it is 4.0h, cyclisation pyrolysis product 920g is obtained altogether.
Embodiment 2
1) by RFFor CF3CF2CF2CF2CH2CH21000 mass parts of polysiloxane oligomers containing chain fluoroalkyl, hydrogen-oxygen
Change 0.5 mass parts of potassium, 15 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and step up
Container contents temperature is cracked, front-end volatiles are steamed；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.97MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 3.5h, obtains cyclisation pyrolysis product 926g altogether.
Embodiment 3
1) by RFFor CF3CF2CF2CF2CH2CH21000 mass parts of polysiloxane oligomers containing chain fluoroalkyl, hydrogen-oxygen
Change 10 mass parts of potassium, 35 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and step up
Container contents temperature is cracked, front-end volatiles are steamed；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.93MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 4.0h, obtains cyclisation pyrolysis product 914g altogether.
Embodiment 4
1) by RFFor CF3CF2CF2CF2CH2CH21000 mass parts of polysiloxane oligomers containing chain fluoroalkyl, hydrogen-oxygen
Change 2 mass parts of potassium, 10 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and step up and split
Container contents temperature is solved, front-end volatiles are steamed；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.90MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 4.5h, obtains cyclisation pyrolysis product 917 altogether.
Embodiment 5
1) by RFFor CF3CF2CF2CF2CH2CH21000 mass parts of polysiloxane oligomers containing chain fluoroalkyl, hydrogen-oxygen
Change 7 mass parts of potassium, 50 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and step up and split
Container contents temperature is solved, front-end volatiles are steamed；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.95MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 3.0h, obtains cyclisation pyrolysis product 933g altogether.
Embodiment 6
1) by RFFor CF3CF2CF2CF2CF2CF2CH2CH21000 mass of polysiloxane oligomers containing chain fluoroalkyl
Part, 5 mass parts of potassium hydroxide, 20 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and by
Step improves cracking container contents temperature, steams front-end volatiles；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.95MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 3.0h, obtains cyclisation pyrolysis product 930g altogether.
Embodiment 7
1) by RFFor CF3CF2CF2C(CF3)2CH2CH2CH21000 mass of polysiloxane oligomers containing chain fluoroalkyl
Part, 5 mass parts of potassium hydroxide, 20 mass parts of octadecyl alcolol are added in cracking container, open stirring, start simultaneously at and vacuumize, and by
Step improves cracking container contents temperature, steams front-end volatiles；
2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking container, while keeping in cracking container
Vacuum degree be -0.95MPa, and continue to step up cracking container contents temperature extraction cracking product, to without product continuation
Extraction.The rectifying time is 4.0h, obtains cyclisation pyrolysis product 927g altogether.
Comparative example 1
It is not passed through inert gas into cracking container using formula same as Example 1, but after isolating front-end volatiles,
Vacuum degree is also maintained at -0.95MPa.The rectifying time is 17h, obtains cyclisation pyrolysis product 734g altogether.
Comparative example 2
It is not passed through inert gas into cracking container using formula same as Example 6, but after isolating front-end volatiles,
Vacuum degree is also maintained at -0.95MPa.The rectifying time is 16h, obtains cyclisation pyrolysis product 725g altogether.
Comparative example 3
In addition to being not added with octadecyl alcolol, remaining formula and technique are same as Example 1.The rectifying time is 6.0h, obtains ring altogether
Change pyrolysis product 843g.
Claims (3)
1. a kind of polysiloxane oligomers cleavage method containing chain fluoroalkyl, which comprises the following steps:
(1) polysiloxane oligomers containing chain fluoroalkyl, catalyst, octadecyl alcolol are added to the cracking reaction kettle of cracker
In, wherein the catalyst be oligomer quality dosage 0.05~1%, the octadecyl alcolol be oligomer quality dosage 1~
5%, stirring is opened, starts simultaneously at and vacuumizes, and steps up cracking container contents temperature, steams front-end volatiles；
(2) after isolating front-end volatiles, start continuously to be passed through inert gas into cracking reaction kettle, while keeping in cracking reaction kettle
Vacuum degree more than -0.9MPa, and continue to step up cracking reaction material temperature in kettle extraction cracking product, up to no production
Product continue to produce, and the rectifying time controls in 2.5~4.5h；
The polysiloxane oligomers formula containing chain fluoroalkyl
It indicates, wherein x, y are the integer more than or equal to 4, RFIndicate that chain fluoroalkyl, Me indicate methyl；The chain fluoroalkyl RF
Formula C can be usednF2n+1(CH2)mIt indicates, the integer that wherein n is 3~8, m is 2 or 3；
The cracker, including cracking reaction kettle (5), insertion tube (3), condenser pipe (7), interior be equipped with of cracking reaction kettle (5) are stirred
It mixes device (12), one end of insertion tube (3) is inserted into cracking reaction kettle by insert port (11) and is connected to gas distributor (4),
The other end is connected to by pipeline (2) with inert gas tank (1), and one end of condenser pipe (7) passes through vacuum pipe (10) and vacuum pump
(9) it is connected, the upper end that the other end receives container (8) and rectifying column (6) with product respectively is connected, and the lower end of rectifying column passes through gas phase
Mouth (13) is connected to cracking reaction kettle (5), and gas distributor (4) and the vertical range of cracking reaction kettle (5) bottom are at least
0.5cm；Cracking reaction kettle (5) is the cracking container that the thermally conductive flow of oil of high-temperature medium is marked in jacket type and collet.
2. cleavage method according to claim 1, it is characterised in that: the R containing chain fluoroalkylFIt is selected from
CF3CF2CF2CF2CH2CH2、CF3CF2CF2CF2CF2CF2CH2CH2、CF3CF2CF2C(CF3)2CH2CH2CH2One of.
3. cleavage method according to claim 1, it is characterised in that: the catalyst is selected from potassium hydroxide, hydroxide
One of sodium, cesium hydroxide, tetramethylammonium hydroxide, potassium carbonate, sodium carbonate, calcium carbonate alkaline compound.
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