CN113321809A - Preparation method of MQ resin with narrow molecular weight distribution - Google Patents
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
Abstract
The invention provides a preparation method of MQ resin with narrow molecular weight distribution, which comprises the following steps: a) sodium silicate and hydrochloric acid aqueous solution are subjected to continuous polymerization reaction in a reactor A to form polysilicic acid hydrosol; b) in the reactor B, continuously adding the product of the reactor A, alcohol, a solvent, an end-capping reagent and an organic silicon additive to carry out end-capping reaction; c) the reactor B product was divided into two phases: an organic phase comprising an MQ resin and an aqueous phase; d) the organic phase containing the MQ resin is purified as MQ resin product in a single solvent system using a continuous rectification process. The MQ resin has the characteristics of continuous production and narrow molecular weight distribution.
Description
Technical Field
The invention relates to a preparation method of silicon resin, in particular to a preparation method of MQ resin with narrow molecular weight distribution.
Background
Silicone is a class of low molecular weight polymers having a three-dimensional network structure. It can be applied to many fields such as adhesives, antifoaming agents, additives, personal care, etc. depending on the structural characteristics.
MQ resins are a special class of silicone resins having monovalent trimethylsilyl (M) units and tetravalent (Q) units. The Q units in MQ resins are usually provided by sodium silicate or silicate esters, and MQ resin processes can be classified into sodium silicate and silicate ester processes, depending on their raw materials. Wherein the sodium silicate is widely applied to the production of MQ resin due to low cost.
US published patent US3772247 provides a synthesis method for preparing MQ resin by a batch process, which aims to provide a synthesis method of low-hydroxyl MQ resin. In order to reduce the hydroxyl content of the MQ resin, the patent adopts a method of trimethyl chlorosilane reflux reaction. US patent publication US9732191 provides a process for the preparation of vinyl MQ resins, which employs vinyl dimethylchlorosilane as a starting material, and terminates the MQ resin into a vinyl terminated product by a reflux reaction. U.S. published patent No. 5837784 provides a method for modifying MQ resin by catalyzing M, D, T units of different structures with basic catalyst to modify MQ resin, thereby improving its application range.
Chinese published patent CN101460543 provides a process technology for preparing MQ resin by a continuous method. The patent uses a power greater than 10kW/m3The strong mixing device solves the problem of rapid mixing in the polycondensation process, and can obtain an MQ resin product with the molecular weight of 8000-13000.
MQ resins can be produced by either batch or continuous processes, and improvements in the range of applications have also been reported by modifying MQ resins, but nothing has been discussed about how to produce narrow molecular weight distribution MQ resins.
Disclosure of Invention
The invention provides a continuous preparation method of narrow molecular weight distribution MQ resin, which can well control the molecular generation process of silicic acid polymerization stage and further control the molecular weight distribution of MQ resin products.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a preparation method of a narrow molecular weight distribution MQ resin comprises the following steps:
a) sodium silicate and hydrochloric acid aqueous solution are subjected to continuous polymerization reaction in a reactor A to form polysilicic acid hydrosol;
b) in the reactor B, continuously adding the product of the reactor A, alcohol, a solvent, an end-capping reagent and an organic silicon additive to carry out end-capping reaction;
c) the reactor B product was divided into two phases: an organic phase comprising an MQ resin and an aqueous phase;
d) the organic phase containing the MQ resin is purified as MQ resin product in a single solvent system using a continuous rectification process.
As a specific embodiment, a process for the preparation of a narrow molecular weight distribution MQ resin, comprising the steps of:
a) the reactor A comprises a static mixing device and an aging reactor, and sodium silicate and hydrochloric acid aqueous solution are subjected to continuous polymerization reaction in the reactor to form polysilicic acid hydrosol;
b) the reactor B carries out end capping reaction by continuously adding the product of the reactor A, alcohol, a solvent, an end capping agent and an organic silicon additive;
c) a phase separator C which separates the product of the reactor B into two phases: an organic phase comprising an MQ resin and an aqueous phase;
d) and the rectifying tower D adopts a continuous rectifying process to purify the organic phase containing the MQ resin into an MQ resin product of a single solvent system.
The principle of the formation of polysilicic acid from aqueous sodium silicate and hydrochloric acid in reactor a can be illustrated by the following two reactions:
the reaction (1) is a fast reaction, and the reaction time is far less than 1 s; reaction 2 is a slow reaction, but reaction (2) reaction rate is affected by temperature, concentration, pH, and the like. Thus, in the present application, a rapid mixing device is selected to effect reaction (1) and an aging reactor is used to effect reaction (2). Therefore, to obtain a satisfactory product, the residence time in the rapid mixing device is less than or equal to 1S, and the residence time in the aging reactor may be 10-120 min.
The rapid mixing device of the present invention employs a static mixer having the following features: selected from SV type, SK type, SX type, SH type and SL type, the unit number is 5-50, and the liquid flow rate is 1-10 m/s; is preferably selected from SK type, SH type and SL type, the unit number is 10-30, and the liquid flow velocity is 2-8 m/s.
Under the condition of determining reaction conditions such as temperature, concentration, pH and the like, the molecular weight distribution of the MQ resin is influenced by the residence time distribution of the reactor, so that a tubular reactor is selected for an aging reactor in the reactor A to ensure that the residence time of all materials is the same, and further the narrow molecular weight distribution of the product is ensured. If a full-mixed flow kettle type reactor is adopted, the molecular weight distribution in the silicic acid polymerization stage is widened due to the existence of a composition with too long or too short residence time because of the residence time distribution brought by the reactor.
In the invention, the temperature of the polymerization reaction in the step a) is selected from 0-30 ℃, the reaction time is 10-120min, and/or, SiO2The molar ratio of the HCl to the HCl is 0.3-0.9.
In the invention, the synthesis process of the MQ resin is a two-phase reaction of an organic phase and a water phase, and in order to improve the reaction efficiency, a solvent is required to be added to improve the compatibility of the product in the organic phase. The invention selects an alcohol as a compatible solvent, and the alcohol can also be used as a stabilizing agent of polysilicic acid. The alcohol in the reactor B is selected from methanol, ethanol, propanol, butanol, isopropanol and isobutanol; preferably one or more selected from ethanol, propanol, butanol, isopropanol; more preferably from ethanol and/or isopropanol. In an amount of 10 wt% to 30 wt%, based on the total amount of feed in reactor B (i.e., the total amount of reactor A product, alcohol, solvent, endblocker, and silicone additive).
Even after the addition of the above-mentioned compatible solvent, a distinct phase interface between the organic and aqueous phases still exists. The reactor B of the invention is added with an organic silicon additive, which can effectively improve the end capping speed and effect of the end capping agent on the polysilicic acid. The effective end capping of polysilicic acid can reduce the non-uniform condensation reaction, thereby achieving the purpose of narrow molecular weight distribution of the product. The organic silicon additive is polyether modified silicone oil, the molecular weight of the organic silicon additive is 1000-4000, and the HLB value of the organic silicon additive is 1-5. The polyether-modified silicone oil can be tailored according to the molecular weight and HLB value, such as polyether-modified silicone oil 1 (molecular weight 2000, HLB value 1.5), polyether-modified silicone oil 2 (molecular weight 3000, HLB value 5), and polyether-modified silicone oil 3 (molecular weight 2000, HLB value 2). In an amount of 0.1 to 5% by weight, based on the total amount of all the raw materials in the reactor B.
The organic solvent in the invention mainly acts as an extracting agent, and effectively extracts the primarily capped MQ resin from a water phase to an organic phase for further capping reaction. The solvent is selected from hexamethyldisiloxane, toluene, xylene, straight-chain alkane and branched-chain alkane. In an amount of 10 to 30% by weight, based on the total amount of all the starting materials in the reactor B.
The reactor B in the invention is a capping reactor, and a full mixed flow kettle type reactor is generally adopted, and the reactor has the function of capping the reaction product polysilicic acid of the reactor A into an MQ resin structure with organic groups. The prolonged residence time in the reactor B leads to the broadening of the molecular weight distribution of the MQ resin product, the too short residence time leads to the incomplete capping reaction, and the product M: Q is too low to meet the application requirements. The invention adopts a mode of improving reaction pressure and temperature, improves end-capping effect, shortens end-capping time and further achieves the aim of narrow molecular weight distribution of products. In the invention, the reaction temperature of the end-capping reactor B is 60-120 ℃, the reaction pressure is 0.1-5bar, and the end-capping time is 30-360 min; preferably, the reaction temperature of the reactor is 70-110 ℃, the reaction pressure is 0.1-3bar, and the end-capping time is 30-180 min.
The Q units in the MQ resin are provided by sodium silicate and the M units are provided by capping agents. The blocking agent in the present invention is selected from the group consisting of trimethylchlorosilane, dimethylchlorosilane, vinyldimethylchlorosilane, hexamethyldisiloxane, tetramethyldisiloxane, divinyltetramethyldisiloxane. In amounts of from 2 to 20% by weight, based on the total amount of all starting materials in reactor B.
The process conditions of the rectifying tower D need to be determined according to the boiling point of the solvent additionally used in the process and the later stage, the rectifying tower adopts normal pressure rectification, and the operating temperature is 10-20 ℃ higher than the boiling point of the solvent.
The invention has the beneficial effects that:
1. compared with the existing batch production process, the process for preparing the MQ resin by the continuous method has the advantages of high product quality stability and high production efficiency.
2. The MQ resin produced by the preparation method of the MQ resin provided by the invention has the characteristic of narrow molecular weight distribution, the number average molecular weight is 1000-20000, and the molecular weight distribution is 1.1-2.5. The molecular weight distribution is superior to that of the common products with the molecular weight distribution of 2-5.
Description of the drawings: FIG. 1 is a graph of molecular weight distribution of example and comparative MQ resin products.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
In the examples, the molecular weight and its distribution were tested: the measurement was carried out by gel chromatography (GPC) using ethyl acetate as a mobile phase, model LC-20AD by GPC apparatus and Shimadzu corporation.
Sources of raw materials in examples: sodium silicate was purchased from lazhou soda ash ltd; the remaining materials were purchased from Sigma-Aldrich.
Preparation methods of polyether-modified silicone oils are well known in the art, and the preparation methods are exemplified by the following (molecular weight 2000, HLB value 1.5):
60g of 2,4,6, 8-tetramethylcyclotetrasiloxane, 1639g of octamethylcyclotetrasiloxane, 162g of hexamethyldisiloxane and 1.8g of trifluoromethanesulfonic acid were put into a 3L four-necked glass flask, and the mixture was stirred at 50 ℃ for reaction for 5 hours. The reaction was neutralized for 1h by adding 12g of calcium carbonate and then filtered to give the crude product. And removing volatile components of the crude product at 120 ℃, under the vacuum degree of 10mbar and for 2 hours to obtain the hydrogen-containing silicone oil.
A500-ml four-necked glass flask was charged with 300g of the above hydrogen-containing silicone oil, 38g of ethylene glycol monoallyl ether, and 0.8g of a Kansted catalyst (Pt content 2000ppm, divinyltetramethyldisiloxane complex), and reacted at 90 ℃ for 2 hours. After the reaction is finished, reducing the vacuum degree of the reaction system to 10mbar, heating to 120 ℃, maintaining for 2 hours, and removing the small molecular compounds to obtain the polyether modified silicone oil with the molecular weight of 2000 and the HLB value of 1.5.
Polyether modified silicone oil with different molecular weights and HLB can be prepared by changing the raw material ratio, the preparation formula of the polyether modified silicone oil in the embodiment 4 is shown in the following table, and the catalyst dosage and the reaction conditions are the same as those in the above example.
Example 1
Mixing 40 w.t% sodium silicate solution (modulus 3.1) and 20 w.t% hydrochloric acid solution at 15 deg.C according to SiO2The reaction was carried out at a molar HCl/HCl ratio of 0.5. The static mixer in the reactor A is an SK type static mixer, the number of units is 20, the flow rate of liquid is 5m/s, and the retention time is 0.4 s. The aging reactor in the reactor A is a tubular reactor, and the retention time is 30 min.
The product from reactor A, isopropanol, hexamethyldisiloxane, trimethylchlorosilane, polyether silicone oil (molecular weight 2000, HLB value 1.5) were continuously fed to reactor B at 87.75kg/h, 20.25kg/h, 6.075kg/h, 0.675kg/h, respectively. The reaction temperature of the reactor B is 80 ℃, the reaction pressure is 1bar, and the end capping reaction time is 120 min. The product from reactor B was sent to a continuous phase separator with a 50min residence time. Finally, the organic phase separated by the phase separator is replaced and rectified by dimethylbenzene at 23kg/h, wherein the rectifying operation temperature is 155 ℃, and the operation pressure is normal pressure. A 70 w.t.% solution of MQ resin in xylene was obtained. The resulting product MQ resin (I) was determined to have a number average molecular weight of 4500 and a molecular weight distribution of 1.4.
Example 2
Mixing 40 w.t% sodium silicate solution (modulus 3.1) and 20 w.t% hydrochloric acid solution at 30 deg.C according to SiO2The reaction was carried out at a molar HCl/HCl ratio of 0.6. The static mixer in the reactor A is SH type static mixer, the number of units is 10, the flow rate of liquid is 8m/s, and the retention time is 0.125 s. The aging reactor in the reactor A is a tubular reactor, and the retention time is 20 min.
The product in the reactor A, isopropanol, xylene, trimethylchlorosilane, vinyl dimethylchlorosilane and polyether silicone oil (molecular weight 4000 and HLB value 5) are continuously added into a reactor B at 87.75kg/h, 13.5kg/h, 10kg/h, 9.57kg/h and 0.675kg/h respectively. The reaction temperature of the reactor B is 70 ℃, the reaction pressure is 0.1bar, and the end capping reaction time is 180 min. The product from reactor B was sent to a continuous phase separator with a residence time of 20 min. Finally, the organic phase separated by the phase separator is supplemented with dimethylbenzene for replacement and rectification at 5kg/h, the rectification operation temperature is 155 ℃, and the operation pressure is normal pressure. A 70 w.t.% solution of MQ resin in xylene was obtained. The resulting product MQ resin (II) was determined to have a number average molecular weight of 12000 and a molecular weight distribution of 1.8.
Example 3
Mixing 40 w.t% sodium silicate solution (modulus 3.1) and 20 w.t% hydrochloric acid solution at 0 deg.C according to SiO2The reaction was carried out at a molar HCl/HCl ratio of 0.8. The static mixer in the reactor A was an SL-type static mixer, the number of units was 30, the liquid flow rate was 3m/s, and the residence time was 1 s. The aging reactor in the reactor A is a tubular reactor, and the retention time is 120 min.
The product in reactor A, ethanol, toluene, hexamethyldisiloxane and polyether silicone oil (molecular weight 1000, HLB value 1) were continuously added to reactor B at 87.75kg/h, 20.25kg/h, 13.5kg/h, 13.36kg/h and 0.135kg/h, respectively. The reaction temperature of the reactor B is 110 ℃, the reaction pressure is 3bar, and the end capping reaction time is 30 min. The product from reactor B was sent to a continuous phase separator with a residence time of 100 min. And finally, supplementing 5kg/h of methylbenzene into the organic phase separated by the phase separator, and then rectifying, wherein the rectifying operation temperature is 140 ℃, and the operation pressure is normal pressure. A 70 w.t.% solution of MQ resin in toluene was obtained. The resulting product MQ resin (III) was determined to have a number average molecular weight of 8600 and a molecular weight distribution of 1.9.
Example 4
Mixing 40 w.t% sodium silicate solution (modulus 3.1) and 20 w.t% hydrochloric acid solution at 10 deg.C according to SiO2The reaction was carried out at a molar HCl/HCl ratio of 0.4. The static mixer in the reactor A is an SK type static mixer, the number of units is 20, the flow rate of liquid is 5m/s, and the retention time is 0.4 s. The aging reactor in the reactor A is a tubular reactor, and the retention time is 10 min.
The product in reactor A, isopropanol, hexamethyldisiloxane, trimethylchlorosilane and polyether silicone oil (molecular weight 2000, HLB value 3) were continuously added to reactor B at 74.25kg/h, 20.25kg/h, 27kg/h, 12.15kg/h and 1.35kg/h, respectively. The reaction temperature of the reactor B is 90 ℃, the reaction pressure is 1.5bar, and the end capping reaction time is 180 min. The product from reactor B was sent to a continuous phase separator with a residence time of 30 min. Finally, the organic phase separated by the phase separator is replaced and rectified by dimethylbenzene at 19kg/h, wherein the rectifying operation temperature is 155 ℃, and the operation pressure is normal pressure. A 70 w.t.% solution of MQ resin in xylene was obtained. The resulting product MQ resin (IV) was determined to have a number average molecular weight of 2300 and a molecular weight distribution of 1.3.
Comparative example 1
350g of 20 w.t.% aqueous hydrochloric acid solution are added to a batch reactor at 10 ℃ and then 306g of 40w.t.% aqueous sodium silicate solution (modulus 3.1) are added to the batch reactor over 2h as SiO2Adding the mixture into a reaction kettle at a HCl/mole ratio of 0.8, and respectively adding 170g of isopropanol, 80g of trimethylchlorosilane and 200g of xylene after finishing the dropwise addition. Keeping the temperature of the reaction kettle at 70 ℃, and continuing the reaction for 2 hours.
After the reaction is finished, stopping stirring, and standing for layering. The lower aqueous phase was removed and the reaction system was distilled at elevated temperature to remove isopropanol, water and hexamethyldisiloxane, yielding a 70 w.t.% solution of MQ resin in xylene. The resulting product MQ resin (V) was determined to have a number average molecular weight of 4800 and a molecular weight distribution of 2.9.
Comparative example 2
Mixing 40 w.t% sodium silicate solution (modulus 3.1) and 20 w.t% hydrochloric acid solution at 10 deg.C according to SiO2The reaction was carried out at a molar HCl/HCl ratio of 0.4. The static mixer in the reactor A is an SK type static mixer, the number of units is 20, the flow rate of liquid is 5m/s, and the retention time is 0.4 s. The aging reactor in the reactor A is a tubular reactor, and the retention time is 10 min.
The product in reactor A, isopropanol, hexamethyldisiloxane, trimethylchlorosilane and polyether silicone oil (molecular weight 500, HLB value 10) were continuously added to reactor B at 74.25kg/h, 20.25kg/h, 27kg/h, 12.15kg/h and 1.35kg/h, respectively. The reaction temperature of the reactor B is 90 ℃, the reaction pressure is 1.5bar, and the end capping reaction time is 180 min. The product from reactor B was sent to a continuous phase separator with a residence time of 30 min. Finally, the organic phase separated by the phase separator is replaced and rectified by dimethylbenzene at 19kg/h, wherein the rectifying operation temperature is 155 ℃, and the operation pressure is normal pressure. A 70 w.t.% solution of MQ resin in xylene was obtained. The resulting product MQ resin (V) was determined to have a number average molecular weight of 2600 and a molecular weight distribution of 1.9.
Claims (9)
1. A preparation method of MQ resin with narrow molecular weight distribution is characterized by comprising the following steps:
a) sodium silicate and hydrochloric acid aqueous solution are subjected to continuous polymerization reaction in a reactor A to form polysilicic acid hydrosol;
b) in the reactor B, continuously adding the product of the reactor A, alcohol, a solvent, an end-capping reagent and an organic silicon additive to carry out end-capping reaction;
c) the reactor B product was divided into two phases: an organic phase comprising an MQ resin and an aqueous phase;
d) the organic phase containing the MQ resin is purified as MQ resin product in a single solvent system using a continuous rectification process.
2. The process of claim 1, wherein the reactor A comprises a static mixing device and an aging reactor; the static mixer is selected from SV type, SK type, SX type, SH type or SL type, the number of units is 5-50, and the liquid flow rate is 1-10 m/s; preferably, the static mixer is selected from SK type, SH type or SL type, the number of units is 10-30, and the liquid flow velocity is 2-8 m/s;
the residence time of the materials in the reaction A is less than or equal to 1S.
3. The method of claim 2, wherein the aging reactor is a tubular reactor;
the retention time of the materials in the aging reactor is 10-120 min.
4. The process according to any one of claims 1 to 3, wherein the polymerization temperature in step a) is selected from 0 to 30 ℃ and the reaction time is 10 to 120min, and/or SiO2The molar ratio of the HCl to the HCl is 0.3-0.9.
5. The process according to any one of claims 1 to 4, wherein in step b), the temperature of the end-capping reaction is 60 to 120 ℃, the reaction pressure is 0 to 5bar, and the end-capping reaction time is 30 to 360 min;
the preferable reaction temperature is 70-110 ℃, the reaction pressure is 0.1-3bar, and the end capping reaction time is 30-180 min.
6. The method according to any one of claims 1 to 5, wherein the alcohol is selected from one or more of methanol, ethanol, propanol, butanol, isopropanol, and isobutanol; preferably one or more selected from ethanol, propanol, butanol, isopropanol; more preferably from ethanol and/or isopropanol, and/or in an amount of from 10% to 30% by weight, based on the total amount of all the starting materials in reactor B.
7. The process of any one of claims 1 to 6, wherein the solvent is selected from one or more of hexamethyldisiloxane, toluene, xylene, linear alkanes, branched alkanes, and/or is used in an amount of 10 to 30 wt.%, based on the total amount of all starting materials in reactor B.
8. The process according to any one of claims 1 to 7, wherein the blocking agent is selected from one or more of trimethylchlorosilane, dimethylchlorosilane, vinyldimethylchlorosilane, hexamethyldisiloxane, tetramethyldisiloxane, divinyltetramethyldisiloxane, and/or is used in an amount of 2 to 20 wt.%, based on the total amount of all starting materials in reactor B.
9. The method according to any one of claims 1 to 7, wherein the silicone additive is a polyether-modified silicone oil having a molecular weight of 1000-4000 and an HLB value of 1-5; and/or in an amount of from 0.1 to 5% by weight, based on the total amount of all starting materials in reactor B.
The MQ resin obtained by the preparation process as claimed in any of claims 1 to 9 having a number average molecular weight of 1000-20000 and a molecular weight distribution of 1.1-2.5; preferably, the number average molecular weight is 2000-15000, and the molecular weight distribution is 1.1-2; more preferably, the number average molecular weight is 2000-15000 and the molecular weight distribution is 1.1-1.8.
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| CN115947943A (en) * | 2021-12-08 | 2023-04-11 | 四川晨光博达新材料有限公司 | MQ silicon resin with ultrahigh vinyl content and preparation method thereof |
| CN114230795A (en) * | 2022-01-14 | 2022-03-25 | 万华化学集团股份有限公司 | Method for continuously preparing controllable high molecular weight MQ resin at low power |
| CN114426667A (en) * | 2022-03-16 | 2022-05-03 | 江西海多化工有限公司 | Continuous preparation system and process method of narrow molecular weight MQ resin |
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