CN109851792A - A kind of preparation process of solid acid catalysis synthesis polysiloxanes - Google Patents
A kind of preparation process of solid acid catalysis synthesis polysiloxanes Download PDFInfo
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Abstract
The invention discloses a kind of preparation processes of solid acid catalysis synthesis polysiloxanes, belong to organosilicon material technical field, to solve the problems, such as that silicone product quality, quality stability difference and catalyst circulation are using complexity in the prior art, and provide a kind of preparation process of solid acid catalysis synthesis polysiloxanes.The present invention is catalyzed by using solid acid catalyst to react, and catalyst is easily separated with product after use, be can be reused several times, small to the corrosivity of equipment；Inorganic membrane retention catalyst is used simultaneously, can effectively avoid residual catalyst fines in product, reduces the generation of by-product, improves product quality and yield, reaction condition is mild, is conducive to inhibit side reaction, while energy saving.
Description
Technical field
The present invention relates to a kind of preparation processes of polysiloxanes, synthesize polysiloxanes more particularly to a kind of solid acid catalysis
Preparation process, belong to organosilicon material technical field.
Background technique
Polysiloxanes has numerous excellent performances, is widely used in fields such as daily chemical product, building and automobiles.Production
The traditional catalyst of polysiloxanes is some strong acid or highly basic, and there are many drawbacks, the corrosion of catalyst for this production technology
Property it is strong, the production efficiency of technique is low, and energy consumption is high, needs to obtain final products, and properties of product by complex process process
It is poor.The surface of solid acid or alkali is distributed a large amount of activated centres, has very high catalytic activity, is widely used in high molecular polymerization
In reaction, when solid acid or alkali as a catalyst, traditional filter type can often make residual catalyst fines in product, lead
Cause product quality decline.
Chinese patent CN 102643427B discloses a kind of using the methanol concentrated solution of anhydrous tetramethylammonium hydroxide as catalyst
The method for producing high purity dimethyl silicone oil, needs to be warming up to 120~135 DEG C of decomposition catalysts, the irritation gas of generation after reaction
Taste is easily mixed into product, limits the application range of product.
Chinese patent CN 101768273B discloses a kind of method for synthesizing polysiloxanes as catalyst using heteropoly acid, instead
After answering, silicone product can be just obtained by the washing removal processes such as catalyst and vacuum distillation dehydration, post-processes work
Skill is complicated.
Nowadays requirement of the market to silicone product quality is higher and higher, and traditional production method has been unable to meet market
Demand in order to promote the stability of product quality, quality, while simplifying the recycling process of catalyst, needs to develop novel
Catalyst and production technology.
Summary of the invention
The main object of the present invention is to solve silicone product quality, quality stability difference and catalyst in the prior art
Complicated problem is recycled, and a kind of preparation process of solid acid catalysis synthesis polysiloxanes is provided.
The purpose of the present invention can reach by using following technical solution:
A kind of preparation process of solid acid catalysis synthesis polysiloxanes, synthetic route are as follows:
Wherein, m=40~60, R expression-H or-CH3；
With high containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4With tetramethyl disiloxane HMM as raw material, in Rare Earth Lanthanum
La is modified WO3/TiO2-ZrO2The lower progress telomerisation of solid acid catalysis effect obtains target product.
Tetramethyl disiloxane HMM could alternatively be hexamethyldisiloxane MM.
Its preparation step is as follows:
Step 1: with high containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4, two silicon of tetramethyl disiloxane HMM or hexamethyl
Oxygen alkane MM makees raw material, in the modified WO of Rare Earth Lanthanum La3/TiO2-ZrO2Solid acid catalysis effect is lower to carry out telomerisation；
Step 2: after reaction, opening outlet valve, make material by inorganic membrane filtration, filtrate, which is delivered in distiller, to be taken off
Except low boiling component, obtained target product is delivered to product storage tank, and low boiling component is applied to subsequent processing；
Step 3: when inorganic membrane resistance is larger, using high pressure nitrogen blowback film surface, keeping the material being attached on film surface de-
It falls, after the completion of filtering, clears up inorganic film tube, recycle catalyst, for the use of lower secondary response；
Step 4: D is measured using gas chromatogram fixative4Conversion ratio calculates target product yield, and compares polysiloxanes
Viscosity before removing low boiling component and after removing low boiling component.
Catalyst the preparation method is as follows:
Step 1: carrier TiO2-ZrO2Preparation
By ZrOCl2It is configured to 0.5mol/L aqueous solution, is slowly added to TiCl by certain mol proportion4Liquid is slow added into
Ammonium hydroxide adjusts pH=7,80 DEG C of stirrings 12h, 110 DEG C of dry 12h, 550 DEG C of roasting 3h, and TiO is made2-ZrO2Composite oxides；
Step 2:La2O3-WO3/TiO2-ZrO2The preparation of catalyst
Lanthanum nitrate is added in ammonium metatungstate aqueous solution by a certain percentage, until completely dissolved, by a certain amount of TiO2-
ZrO2Composite oxide power is added in above-mentioned aqueous solution, and 12h, 110 DEG C of dryings are stirred in 80 DEG C, 40kHz ultrasound environments
12h, 700 DEG C of roasting 3h, obtains the xLa of different La load capacity2O3-yWO3/TiO2-ZrO2Catalyst；
Wherein, x indicates that the quality of La accounts for WO3/TiO2-ZrO2The percentage of gross mass；
Y indicates WO3Quality account for TiO2-ZrO2The percentage of carrier quality.
Catalyst is La2O3-WO3/TiO2-ZrO2, wherein the molar ratio of Ti and Zr is 1:1, WO3Content be TiO2-
ZrO2The load capacity of 10%~30%, La of carrier quality is 0.3%~1.0%.
Inoranic membrane membrane tube is the zirconium oxide or Alumina Inorganic membrane tube of average pore size 10nm~3um.
High containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4Mass ratio between tetramethyl disiloxane HMM is 0.0~
3.5:9.5~31.5:1.0.
High containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4Mass ratio between hexamethyldisiloxane MM is 0.0~
3.5:9.5~31.5:1.0.
Telomerisation temperature is 40~70 DEG C.
Removing low boiling component temperature is 140~160 DEG C, vacuum degree -0.09~-0.10MPa.
Advantageous effects of the invention:
The catalyst that the present invention uses is solid acid, and catalyst is easily separated with product after use, be can be reused several times,
It is small to the corrosivity of equipment；Using inorganic membrane retention catalyst, residual catalyst fines in product can be effectively avoided,
The generation of by-product is reduced, improves product quality and yield, reaction condition is mild, is conducive to inhibit side reaction, same to time
About energy consumption.
Detailed description of the invention
Fig. 1 is the process flow diagram that the present invention synthesizes polysiloxanes using solid acid catalysis；
In figure: 1- reaction kettle, 2- valve, 3- pump, 4- inorganic film tube, 5- distiller, 6- product storage tank.
Specific embodiment
To make the more clear and clear technical solution of the present invention of those skilled in the art, the present invention is made below further
Detailed description, embodiments of the present invention are not limited thereto.
As shown in Figure 1, a kind of preparation process of solid acid catalysis synthesis polysiloxanes, with high containing hydrogen silicone oil HS, prestox
Cyclotetrasiloxane D4With tetramethyl disiloxane HMM as raw material, in the modified WO of Rare Earth Lanthanum La3/TiO2-ZrO2Solid acid catalysis
The lower progress telomerisation of effect obtains target product, and raw material and catalyst are added in reaction kettle 1, adjusted at a certain temperature
Poly- balanced reaction opens outlet valve 2-1 after reaction, filters material by inoranic membrane 4 by pumping 3-1, filtrate enters distillation
Low boiling component is removed in device 5, gained target product is delivered to product storage tank 6, when inorganic membrane resistance is larger, opens valve 2-
2, using high pressure nitrogen blowback inoranic membrane.
Embodiment 1:
(1) carrier TiO2-ZrO2Preparation
By ZrOCl2It is configured to 0.5mol/L aqueous solution, Ti:Zr=1:1 is slowly added to TiCl in molar ratio4Liquid, then delay
The slow ammonium hydroxide that is added adjusts pH=7,80 DEG C of stirrings 12h, 110 DEG C of dry 12h, 550 DEG C of roasting 3h, and TiO is made2-ZrO2Combined oxidation
Object.
(2)La2O3-WO3/TiO2-ZrO2The preparation of catalyst
La:W:Zr=0.0101:0.1314:1.0 in molar ratio lanthanum nitrate is added in ammonium metatungstate aqueous solution, to complete
After fully dissolved, by a certain amount of TiO2-ZrO2Above-mentioned aqueous solution is added in composite oxide power, in 80 DEG C and 40kHz ultrasound environments
Middle stirring 12h obtains 0.6%La in 110 DEG C of dry 12h, 700 DEG C of roasting 3h2O3- 15%WO3/TiO2-ZrO2Catalyst.
(3) catalytic performance test
HS:D in mass ratio4: the feedstock transportation of metering into reaction kettle 1, is stirred and is added by HMM=0.0:18.78:1.0
The 0.6%La that material quality score is 1.0% is added to 40 DEG C in heat2O3- 15%WO3/TiO2-ZrO2Catalyst starts to react, instead
After answering, outlet valve 2-1 to be opened, material is delivered to inorganic film tube 4 by pump 3-1 and is filtered, filtrate is delivered in distiller 5,
At 140~160 DEG C of temperature, low boiling component is removed under the conditions of vacuum degree -0.09~-0.10MPa, obtained target product is by pumping
3-2 is delivered to product storage tank 6, and the low boiling component of removing enters subsequent processing through valve 2-4；When inorganic membrane resistance is larger
(filtrate discharge rate reduces to 1/4) opens valve 2-2, using high pressure nitrogen blowback film surface, keeps the material being attached on film surface de-
It falls.After the completion of filtering, inorganic film tube is cleared up, recycles catalyst, for the use of lower secondary response.
D is measured using gas chromatogram fixative4Conversion ratio is 95.4%, and calculating target product yield is 86.4%.Removing
The viscosity of polysiloxanes is 29.3mPas before low boiling component, and the viscosity after removing low boiling component is 41.1mPas (viscous
Degree is 25 DEG C of measurements, similarly hereinafter).
Embodiment 2:
The preparation method of solid acid carrier and catalyst is same as Example 1.
Catalytic performance test: HS:D in mass ratio4: HMM=0.57:9.92:1.0 is by the feedstock transportation of metering to reaction kettle
In 1,40 DEG C are stirred and heated to, the 0.6%La that material quality score is 1.0% is added2O3- 15%WO3/TiO2-ZrO2Catalysis
Agent starts to react, and after reaction, opens outlet valve 2-1, and material is delivered to inorganic film tube 4 by pump 3-1 and is filtered, filtrate conveying
Into distiller 5, at 140~160 DEG C of temperature, low boiling component is removed under the conditions of vacuum degree -0.09~-0.10MPa, is obtained
Target product is delivered to product storage tank 6 by pumping 3-2, and the low boiling component of removing enters subsequent processing through valve 2-4；Work as inoranic membrane
When resistance is larger, open valve 2-2 makes the material being attached on film surface fall off using high pressure nitrogen blowback film surface.Filtering is completed
Afterwards, inorganic film tube is cleared up, catalyst is recycled, for the use of lower secondary response.
D is measured using gas chromatogram fixative4Conversion ratio is 96.2%, and calculating target product yield is 82.3%.Removing
The viscosity of polysiloxanes is 15.0mPas before low boiling component, and the viscosity after removing low boiling component is 21.5mPas.
Embodiment 3:
The preparation method of solid acid carrier and catalyst is same as Example 1.
Catalytic performance test: HS:D in mass ratio4: HMM=2.47:15.98:1.0 extremely reacts the feedstock transportation of metering
In kettle 1,50 DEG C are stirred and heated to, the 0.6%La that material quality score is 1.0% is added2O3- 15%WO3/TiO2-ZrO2It urges
Agent starts to react, and after reaction, opens outlet valve 2-1, and material is delivered to inorganic film tube 4 by pump 3-1 and is filtered, filtrate is defeated
It send into distiller 5, at 140~160 DEG C of temperature, low boiling component is removed under the conditions of vacuum degree -0.09~-0.10MPa, is obtained
Target product by pump 3-2 be delivered to product storage tank 6, the low boiling component of removing enters subsequent processing through valve 2-4；When inorganic
When membrane resistance is larger, open valve 2-2 makes the material being attached on film surface fall off using high pressure nitrogen blowback film surface.It has filtered
Cheng Hou clears up inorganic film tube, recycles catalyst, for the use of lower secondary response.
D is measured using gas chromatogram fixative4Conversion ratio is 95.1%, and calculating target product yield is 85.5%.Removing
The viscosity of polysiloxanes is 28.3mPas before low boiling component, and the viscosity after removing low boiling component is 37.6mPas.
Embodiment 4:
The preparation method of solid acid carrier and catalyst is same as Example 1.
Catalytic performance test: HS:D in mass ratio4: MM=3.30:29.92:1.0 is by the feedstock transportation of metering to reaction kettle
In 1,60 DEG C are stirred and heated to, the 0.6%La that material quality score is 1.0% is added2O3- 15%WO3/TiO2-ZrO2Catalysis
Agent starts to react, and after reaction, opens outlet valve 2-1, and material is delivered to inorganic film tube 4 by pump 3-1 and is filtered, filtrate conveying
Into distiller 5, at 140~160 DEG C of temperature, low boiling component is removed under the conditions of vacuum degree -0.09~-0.10MPa, is obtained
Target product is delivered to product storage tank 6 by pumping 3-2, and the low boiling component of removing enters subsequent processing through valve 2-4；Work as inoranic membrane
When resistance is larger, open valve 2-2 makes the material being attached on film surface fall off using high pressure nitrogen blowback film surface.Filtering is completed
Afterwards, inorganic film tube is cleared up, catalyst is recycled, for the use of lower secondary response.
D is measured using gas chromatogram fixative4Conversion ratio is 94.8%, and calculating target product yield is 88.3%.Removing
The viscosity of polysiloxanes is 59.4 mPas before low boiling component, and the viscosity after removing low boiling component is 78.9mPas.
Embodiment 5:
La:W:Zr=0.0046:0.0438:1.0 in molar ratio prepares solid acid catalyst using the method for embodiment 1
0.3%La2O3- 5%WO3/TiO2-ZrO2。
According to the material quality of embodiment 3, when method evaluates the catalytic performance of above-mentioned catalyst.
D is measured using gas chromatogram fixative4Conversion ratio is 95.5%, and calculating target product yield is 84.8%.Removing
The viscosity of polysiloxanes is 27.7mPas before low boiling component, and the viscosity after removing low boiling component is 37.4mPas.
Embodiment 6:
La:W:Zr=0.0190:0.2628:1.0 in molar ratio prepares solid acid catalyst using the method for embodiment 1
1.0%La2O3- 30%WO3/TiO2-ZrO2。
According to the material quality of embodiment 3, when method evaluates the catalytic performance of above-mentioned catalyst.
D is measured using gas chromatogram fixative4Conversion ratio is 95.1%, and calculating target product yield is 86.1%.Removing
The viscosity of polysiloxanes is 29.3mPas before low boiling component, and the viscosity after removing low boiling component is 38.2mPas.
In the present embodiment, with high containing hydrogen silicone oil (HS), octamethylcy-clotetrasiloxane (D4) and tetramethyl disiloxane
(HMM) or hexamethyldisiloxane (MM) makees raw material, in Rare Earth Lanthanum (La) modified WO3/TiO2-ZrO2Under solid acid catalysis effect
It carries out telomerisation and synthesizes polysiloxanes, by inorganic membrane filtration, filtrate is delivered in distiller to be taken off material after reaction
Except low boiling component, obtained target product is delivered to product storage tank, and low boiling component is applied to subsequent processing, when inoranic membrane hinders
When power is larger, using high pressure nitrogen blowback film surface, the material being attached on film surface is made to fall off, after the completion of filtering, clears up inoranic membrane
Pipe recycles catalyst, and for the use of lower secondary response, technique of the invention overcomes suspended state catalyst and is difficult to the problem of separating,
Residual catalyst fines in product are avoided, are conducive to inhibit side reaction, Improving The Quality of Products, and solid acid used
Catalytic activity it is high, reaction condition is mild, the high-quality polysiloxanes low to production acid value, transparency is high, by-products content is low
It is of great significance.
The above, further embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, and it is any
Within the scope of the present disclosure, according to the technique and scheme of the present invention and its design adds those familiar with the art
With equivalent substitution or change, protection scope of the present invention is belonged to.
Claims (10)
1. a kind of preparation process of solid acid catalysis synthesis polysiloxanes, which is characterized in that synthetic route is as follows:
Wherein, m=40~60, R expression-H or-CH3；
With high containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4With tetramethyl disiloxane HMM as raw material, change in Rare Earth Lanthanum La
Property WO3/TiO2-ZrO2The lower progress telomerisation of solid acid catalysis effect obtains target product.
2. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 1, which is characterized in that tetramethyl
Base disiloxane HMM could alternatively be hexamethyldisiloxane MM.
3. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 2, which is characterized in that it is made
It is standby that steps are as follows:
Step 1: with high containing hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4, tetramethyl disiloxane HMM or hexamethyldisiloxane
MM makees raw material, in the modified WO of Rare Earth Lanthanum La3/TiO2-ZrO2Solid acid catalysis effect is lower to carry out telomerisation；
Step 2: after reaction, open outlet valve, make material by inorganic membrane filtration, filtrate be delivered in distiller remove it is low
Boiling point component, obtained target product are delivered to product storage tank, and low boiling component is applied to subsequent processing；
Step 3: when inorganic membrane resistance is larger, using high pressure nitrogen blowback film surface, so that the material being attached on film surface is fallen off, mistake
After the completion of filter, inorganic film tube is cleared up, recycles catalyst, for the use of lower secondary response；
Step 4: D is measured using gas chromatogram fixative4Conversion ratio calculates target product yield, and compares polysiloxanes and removing
Viscosity before low boiling component and after removing low boiling component.
4. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that catalysis
Agent the preparation method is as follows:
Step 1: carrier TiO2-ZrO2Preparation
By ZrOCl2It is configured to 0.5mol/L aqueous solution, is slowly added to TiCl by certain mol proportion4Liquid is slow added into ammonium hydroxide
PH=7,80 DEG C of stirrings 12h, 110 DEG C of dry 12h, 550 DEG C of roasting 3h are adjusted, TiO is made2-ZrO2Composite oxides；
Step 2:La2O3-WO3/TiO2-ZrO2The preparation of catalyst
Lanthanum nitrate is added in ammonium metatungstate aqueous solution by a certain percentage, until completely dissolved, by a certain amount of TiO2-ZrO2It is multiple
It closes oxide powder to be added in above-mentioned aqueous solution, stirs 12h, 110 DEG C of dry 12h in 80 DEG C, 40kHz ultrasound environments, 700 DEG C
3h is roasted, the xLa of different La load capacity is obtained2O3-yWO3/TiO2-ZrO2Catalyst；
Wherein, x indicates that the quality of La accounts for WO3/TiO2-ZrO2The percentage of gross mass；
Y indicates WO3Quality account for TiO2-ZrO2The percentage of carrier quality.
5. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that catalysis
Agent is La2O3-WO3/TiO2-ZrO2, wherein the molar ratio of Ti and Zr is 1:1, WO3Content be TiO2-ZrO2Carrier quality
The load capacity of 10%~30%, La are 0.3%~1.0%.
6. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that inorganic
Film membrane tube is the zirconium oxide or Alumina Inorganic membrane tube of average pore size 10nm~3um.
7. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that Gao Han
Hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4Mass ratio between tetramethyl disiloxane HMM be 0.0~3.5:9.5~
31.5:1.0.
8. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that Gao Han
Hydrogen silicone oil HS, octamethylcy-clotetrasiloxane D4Mass ratio between hexamethyldisiloxane MM be 0.0~3.5:9.5~
31.5:1.0.
9. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that telomerization
Reaction temperature is 40~70 DEG C.
10. a kind of preparation process of solid acid catalysis synthesis polysiloxanes according to claim 3, which is characterized in that de-
Except low boiling component temperature is 140~160 DEG C, vacuum degree -0.09~-0.10MPa.
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| CN111234227A (en) * | 2020-03-07 | 2020-06-05 | 江西赣江新区有机硅创新研究院有限公司 | Low-molecular-weight methyl silicone oil and preparation method thereof |
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| CN111234227A (en) * | 2020-03-07 | 2020-06-05 | 江西赣江新区有机硅创新研究院有限公司 | Low-molecular-weight methyl silicone oil and preparation method thereof |
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