CN115368400A - Process for recovering organic silicon ring body from silicon rubber series substances - Google Patents
Process for recovering organic silicon ring body from silicon rubber series substances Download PDFInfo
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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 Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention relates to the technical field of silicone rubber recovery, in particular to a process for recovering an organic silicon ring body from silicone rubber series substances. The method comprises the following steps: mixing silicon rubber and an organic solvent, and adding an alkaline catalyst to dissolve the silicon rubber at the reflux temperature of the organic solvent to obtain the organic silicon ring body. In the prior art, the reactions for recovering the silicon rubber are all acidic. The corrosion to the equipment is large, which increases the cost of replacing the equipment and also causes great potential safety hazard in the process of replacing the equipment. Compared with the prior art, the process of recovering the silicon rubber is alkaline, so that the corrosion to equipment is effectively reduced, the cost brought by equipment replacement is reduced on one hand, and potential safety hazards are reduced on the other hand. Meanwhile, acid sludge and solid waste are not generated, and resource waste and environmental pollution are reduced.
Description
Technical Field
The invention relates to the technical field of silicone rubber recovery, in particular to a process for recovering an organic silicon ring body from silicone rubber series substances.
Background
The silicon rubber is a synthetic rubber taking a silicon-oxygen bond as a main chain, has excellent heat resistance, cold resistance, dielectricity, ozone resistance and aging resistance, and is widely applied to various fields. The silicon rubber products are mainly divided into three categories, namely high-temperature rubber, room-temperature rubber and liquid silicon rubber, and the application field is very wide. With the development of the current society and the improvement of the economic level, the consumption of silicon rubber products is continuously increased, the silicon rubber waste products and leftover materials generated in the forming processing and the waste silicon rubber formed after the application are rapidly increased, if the waste silicon rubber is not recycled, the space is occupied, and the resources and the environment are wasted.
At present, the recovery methods of silicon rubber leftover materials and waste products mainly comprise two physical and chemical methods. The physical method for recycling mainly uses the waste silicon rubber as a general filler to be used as a modified filler of rubber, plastics and the like, thereby achieving the purposes of reducing the product cost, reducing the power consumption and modifying. The utilization of the new type of the waste oil is low in economic added value, and certain resource waste is caused.
The chemical method recovery mainly adopts an acid catalytic cracking method at present, and in CN104017366B & lt & gt Silicone rubber cracking recovery regeneration technology & gt, the adopted acid is concentrated sulfuric acid and the temperature is 170-230 ℃ for cracking. The corrosion to equipment is obvious due to the high-temperature strong acid; in CN 113563376A, a method for recovering waste silicone rubber, alkali metal is adopted, the process is carried out at high temperature and high pressure of 3-5Mpa, and the obtained product is still rearranged with dilute sulphuric acid at high temperature of 140-150 ℃; the corrosion of acid to equipment can not be avoided; in the method of CN 105860129B method for cracking and recovering organosilicon micromolecules and ring bodies of silicon rubber series substances, an organosilicon halogenating agent is used for breaking a main chain, then polysiloxane with a chlorine bond is subjected to back-biting reaction, and the organosilicon ring bodies are obtained through rearrangement; the adoption of organic silicon halide and the artificial introduction of a large amount of chlorine element cause corrosion to equipment, potential safety hazard and environmental pollution, and is not an ideal route. Therefore, the method adopts high-temperature strong acid in the multi-acid method cracking process in the prior acid method cracking, which has the problems of serious corrosion to equipment, need of regular replacement, potential safety hazard and high cost. Meanwhile, more acid sludge and solid waste are generated after cracking is finished, so that resource waste and environmental pollution are caused.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a process for recovering an organic silicon ring body from a silicon rubber series substance.
In order to solve the technical problems, the invention provides the following technical scheme:
a process for recovering organosilicon cyclic body from silicone rubber series substances comprises the following steps: mixing silicon rubber and an organic solvent, and adding an alkaline catalyst to dissolve the silicon rubber at the reflux temperature of the organic solvent to obtain the organic silicon ring body.
In practical application, the silicone rubber is a network structure with a silicone-oxygen chain as a main chain. When the silicon rubber is mixed in an organic solvent and the alkaline catalyst is added at the reflux temperature of the organic solvent, the alkaline catalyst destroys the silicon-oxygen chain of the silicon rubber, so that the network structure of the silicon rubber is broken into silicon-oxygen chain micromolecules which contain organosilicon ring bodies, and the silicon rubber can be produced again by taking the organosilicon ring bodies as raw materials. Therefore, the invention can effectively recycle the waste silicon rubber, and the recycled product can be put into the production of the silicon rubber again. Meanwhile, the invention reacts in an alkaline environment, can effectively avoid the corrosion of an acidic environment to equipment, and on one hand, the equipment does not need to be replaced periodically, thereby reducing the cost for replacing the equipment and reducing the potential safety hazard when the equipment is replaced. On the other hand, acid sludge and solid waste are not generated in the process, so that the waste of resources and environmental pollution are reduced.
Further, the method comprises the following steps:
a crushing step: pulverizing silicone rubber to obtain silicone rubber particles;
a dissolving step: adding silicon rubber particles and an organic solvent into a reaction kettle, adding an alkaline catalyst at the reflux temperature of the organic solvent to dissolve the silicon rubber particles to obtain a dissolved solution, wherein the dissolved solution contains a crude organosilicon cyclic body;
a purification step: rearranging and rectifying the dissolved solution to obtain fine organosilicon ring bodies.
Further, the "pulverizing step" further comprises the following steps:
washing and drying the silicone rubber to obtain a clean material;
the clean material was crushed and sieved to obtain silicone rubber particles.
Further, the "purification step" further comprises the following steps:
adding water into the reaction kettle to obtain a mixed solution;
distilling the mixed solution under reduced pressure to separate the organic solvent;
after the mixed solution is subjected to reduced pressure distillation, the mixed solution is rearranged and rectified to obtain fine organosilicon ring bodies.
Further, the rearrangement and rectification of the mixed solution to obtain the fine organosilicon ring bodies after the mixed solution is subjected to reduced pressure distillation further comprises the following steps:
after the mixed solution is subjected to reduced pressure distillation, standing the mixed solution until the mixed solution is layered;
after the mixed solution is layered, obtaining an upper oil phase of the mixed solution, and rearranging and rectifying the upper oil phase to obtain a fine organic silicon ring body;
and (3) obtaining a lower water phase of the mixed solution, and carrying out adsorption filtration on the lower water phase to obtain a silicate aqueous solution.
Further, the pH of the water is neutral or weakly alkaline.
Further, the mass ratio of water to the dissolution liquid is 0.4.
Further, the mass ratio of the silicone rubber to the organic solvent is 30:100 to 100:30, of a nitrogen-containing gas; the mass of the alkaline catalyst accounts for 3-15% of the mass of the silicon rubber.
Further, the organic solvent comprises one or more of a one-carbon alcohol, a two-carbon alcohol, a three-carbon alcohol, a five-carbon alkanol, a six-carbon alkanol, a cycloalkane, dimethylamine, diethylamine, triethylamine, pentane, acetone, and tetrahydrofuran.
Further, the alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
Compared with the prior art, the invention has the following advantages:
the invention can effectively recover silicon rubber series substances, obtain the recovered product of the organic silicon ring body, and the obtained organic silicon ring body can be put into the production of the silicon rubber product again.
The reaction environment of the invention is alkaline, thus effectively reducing the corrosion to the equipment, and on one hand, the equipment does not need to be replaced periodically, thereby reducing the cost for replacing the equipment and reducing the potential safety hazard when the equipment is replaced. On the other hand, acid sludge and solid waste are not generated in the process, so that the waste of resources and environmental pollution are reduced.
The invention can obtain a byproduct silicate aqueous solution, and the obtained silicate aqueous solution can be put into the production of other products, which is equivalent to the recovery of inorganic silicon in silicon rubber.
Drawings
FIG. 1: the overall flow chart.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
The first embodiment is as follows:
a process for recovering organosilicon cyclic body from silicone rubber series substances comprises the following steps: a crushing step, a dissolving step and a purifying step. Specifically, the crushing step comprises: washing and drying the silicone rubber to obtain a clean material, crushing the clean material, and sieving the crushed clean material by using a screen with the mesh number of 10-100 to obtain silicone rubber particles. Wherein the microstructure of the silicon rubber is a net structure taking a silicon-oxygen chain as a main chain. Specifically, the silicone rubber may be one or more of a waste silicone rubber product, a silicone rubber mixed rubber, a raw silicone rubber, a mixed rubber of the silicone rubber and other rubbers, a graft copolymer of the silicone rubber and other compounds, a block copolymer of the silicone rubber and other compounds, an organic silicon adhesive, an organic silicon coating, and a silicone resin.
The dissolving step comprises: adding the obtained silicone rubber particles and an organic solvent into a reaction kettle together, wherein the mass ratio of the silicone rubber particles to the organic solvent is 30. The basic catalyst is added at the reflux temperature of the organic solvent. The mass of the alkaline catalyst accounts for 3 percent of the mass of the silicon rubber particles. After the alkaline catalyst is added, the alkaline catalyst can destroy silica chains of the silicon rubber particles under the current environment, so that the network structure of the silicon rubber is broken into silica chain small molecules, and in the silica chain small molecules, one part is a straight chain and the other part is an organosilicon ring body. The obtained siloxane chain small molecules are mixed into an organic solvent. Thus, a crude silicone ring body is obtained. At this time, the silicone rubber particles are dissolved in an organic solvent, and mixed with the organic solvent to form a dissolved solution. Meanwhile, in actual production, a part of inorganic silicon is added in the silicone rubber for reinforcement, and the inorganic silicon and the alkaline catalyst coexist in an organic solvent. Wherein the organic solvent comprises one or more of monohydric alcohol, dihydric alcohol, trihydric alcohol, pentahydric alcohol, hexahydric alcohol, cycloalkane, dimethylamine, diethylamine, triethylamine, pentane, acetone and tetrahydrofuran. The alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
The purification step comprises: water was added to the reaction kettle to obtain a mixed solution. Wherein the pH value of the water is neutral or alkalescent. The mass ratio of water to the dissolution liquid was 0.4. When water is added, the water body is alkaline after the water is added because the alkaline catalyst is alkaline, and the inorganic silicon reacts in the alkaline water body to generate silicate. At this time, the silicate dissolves into water to become a silicate aqueous solution. Stirring the mixed solution, and distilling the mixed solution under reduced pressure at 50mbar and 50 deg.C to separate the organic solvent from the dissolved solution. After the mixture was distilled under reduced pressure, the mixture was allowed to stand to allow the mixture to separate into layers. And (3) taking the upper oil phase of the mixed solution for rearrangement rectification, wherein the temperature of the rearrangement rectification is 150 ℃. After rearrangement and rectification, refined organosilicon ring bodies can be obtained. The obtained silicone ring body can be put into production of products related to silicone rubber again. Taking the lower water phase of the mixed solution, and adsorbing and filtering the lower water phase to separate the silicate aqueous solution.
In conclusion, the invention can effectively recover silicon rubber series substances, and the recovered organic silicon ring body can be put into the production of silicon rubber products again. On the other hand, the reaction environment of the invention is alkaline, and the corrosion of the acid environment to the equipment can be effectively avoided, so that the equipment does not need to be replaced periodically, the cost for replacing the equipment is reduced, and the potential safety hazard when the equipment is replaced is reduced. And acid sludge and solid waste are not generated in the process, so that the waste of resources and environmental pollution are reduced. Meanwhile, the invention can produce by-product silicate aqueous solution in the reaction process, can be put into the production of other products, and is equivalent to the recovery of inorganic silicon used for reinforcement in silicon rubber.
Example two:
the crushing step comprises: washing and drying the silicone rubber to obtain a clean material, crushing the clean material, and sieving the crushed clean material by using a screen with the mesh number of 10-100 to obtain silicone rubber particles. Specifically, the silicone rubber may be one or more of a waste silicone rubber product, a silicone rubber mixed rubber, a raw silicone rubber, a mixed rubber of the silicone rubber and other rubbers, a graft copolymer of the silicone rubber and other compounds, a block copolymer of the silicone rubber and other compounds, an organic silicon adhesive, an organic silicon coating, and a silicone resin.
The dissolving step comprises: adding the obtained silicone rubber particles and an organic solvent into a reaction kettle together, wherein the mass ratio of the silicone rubber particles to the organic solvent is 60. The basic catalyst is added at the reflux temperature of the organic solvent. The mass of the alkaline catalyst accounts for 8 percent of the mass of the silicon rubber particles. After the alkaline catalyst is added, the silicone rubber particles are dissolved in the organic solvent and mixed with the organic solvent to form a solution containing the organosilicon ring bodies. Wherein the organic solvent comprises one or more of monohydric alcohol, dihydric alcohol, trihydric alcohol, pentahydric alcohol, hexahydric alcohol, cycloalkane, dimethylamine, diethylamine, triethylamine, pentane, acetone and tetrahydrofuran. The alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
The purification step comprises: water was added to the reaction kettle to obtain a mixed solution. Wherein the pH value of the water is neutral or alkalescent. The mass ratio of water to the dissolution liquid was 0.6. The mixture was stirred and distilled under reduced pressure at a vacuum of 50mbar and a temperature of 55 ℃ to separate the organic solvent from the dissolved solution. After the mixture was distilled under reduced pressure, the mixture was allowed to stand to allow the mixture to separate into layers. And (3) taking the upper oil phase of the mixed solution for rearrangement rectification, wherein the temperature of the rearrangement rectification is 170 ℃. After rearrangement and rectification, refined organosilicon ring bodies can be obtained. The obtained silicone ring body can be put into production of products related to silicone rubber again. Taking the lower aqueous phase of the mixed solution, and adsorbing and filtering the lower aqueous phase to separate the silicate aqueous solution.
Example three:
the crushing step comprises: washing and drying the silicone rubber to obtain a clean material, crushing the clean material, and sieving the crushed clean material by using a screen with the mesh number of 10-100 to obtain silicone rubber particles. Specifically, the silicone rubber may be one or more of a waste silicone rubber product, a silicone rubber mixed rubber, a raw silicone rubber, a mixed rubber of the silicone rubber and other rubbers, a graft copolymer of the silicone rubber and other compounds, a block copolymer of the silicone rubber and other compounds, an organic silicon adhesive, an organic silicon coating, and a silicone resin.
The dissolving step comprises: adding the obtained silicone rubber particles and an organic solvent into a reaction kettle together, wherein the mass ratio of the silicone rubber particles to the organic solvent is 2:1. The basic catalyst is added at the reflux temperature of the organic solvent. The mass of the alkaline catalyst accounts for 12 percent of the mass of the silicon rubber particles. After the alkaline catalyst is added, the silicone rubber particles are dissolved in the organic solvent and mixed with the organic solvent to form a solution containing the organosilicon ring bodies. Wherein the organic solvent comprises one or more of monohydric alcohol, dihydric alcohol, trihydric alcohol, pentahydric alcohol, hexahydric alcohol, cycloalkane, dimethylamine, diethylamine, triethylamine, pentane, acetone and tetrahydrofuran. The alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
The purification step comprises: water was added to the reaction kettle to obtain a mixed solution. Wherein the pH value of the water is neutral or alkalescent. The mass ratio of water to the dissolution liquid was 0.8. The mixture was stirred and distilled under reduced pressure at a vacuum of 50mbar and a temperature of 60 ℃ to separate the organic solvent from the dissolved solution. After the mixture was distilled under reduced pressure, the mixture was allowed to stand to allow the mixture to separate into layers. And (3) taking the upper oil phase of the mixed solution for rearrangement rectification, wherein the temperature of the rearrangement rectification is 200 ℃. After rearrangement and rectification, refined organosilicon ring bodies can be obtained. The silicone rings obtained can be used again in the production of products relating to silicone rubbers. Taking the lower aqueous phase of the mixed solution, and adsorbing and filtering the lower aqueous phase to separate the silicate aqueous solution.
Example four:
the crushing step comprises: washing and drying the silicone rubber to obtain a clean material, crushing the clean material, and sieving the crushed clean material by using a screen with the mesh number of 10-100 to obtain silicone rubber particles. Specifically, the silicone rubber can be one or more of waste silicone rubber products, silicone rubber mixed rubber, raw silicone rubber, blended rubber of silicone rubber and other rubber, graft copolymer of silicone rubber and other compounds, block copolymer of silicone rubber and other compounds, silicone adhesive, silicone coating and silicone resin.
The dissolving step comprises: adding the obtained silicon rubber particles and an organic solvent into a reaction kettle together, wherein the mass ratio of the silicon rubber particles to the organic solvent is 100:30. the basic catalyst is added at the reflux temperature of the organic solvent. The mass of the alkaline catalyst accounts for 15% of the mass of the silicone rubber particles. After the alkaline catalyst is added, the silicone rubber particles are dissolved in an organic solvent and mixed with the organic solvent to form a solution containing the organosilicon cyclic bodies. Wherein the organic solvent comprises one or more of monohydric alcohol, dihydric alcohol, trihydric alcohol, pentahydric alcohol, hexahydric alcohol, cycloalkane, dimethylamine, diethylamine, triethylamine, pentane, acetone and tetrahydrofuran. The alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
The purification step comprises: water was added to the reaction kettle to obtain a mixed solution. Wherein the pH value of the water is neutral or alkalescent. The mass ratio of water to the dissolution solution was 1:1. The mixture was stirred and distilled under reduced pressure at a vacuum of 50mbar and a temperature of 70 ℃ to separate the organic solvent from the dissolved solution. After the mixture was distilled under reduced pressure, the mixture was allowed to stand to allow the mixture to separate into layers. And (3) taking the upper oil phase of the mixed solution for rearrangement rectification, wherein the temperature of the rearrangement rectification is 230 ℃. After rearrangement and rectification, refined organosilicon ring bodies can be obtained. The obtained silicone ring body can be put into production of products related to silicone rubber again. Taking the lower aqueous phase of the mixed solution, and adsorbing and filtering the lower aqueous phase to separate the silicate aqueous solution.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments, or alternatives may be employed, by those skilled in the art, without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. A process for recovering organic silicon rings from silicon rubber series substances is characterized by comprising the following steps: the method comprises the following steps: mixing silicon rubber and an organic solvent, and adding an alkaline catalyst to dissolve the silicon rubber at the reflux temperature of the organic solvent to obtain the organic silicon ring body.
2. The process for recovering silicone rings from silicone rubber series substances according to claim 1, wherein the process comprises the following steps: the method comprises the following steps:
a crushing step: pulverizing the silicone rubber to obtain the silicone rubber particles;
a dissolving step: adding the silicon rubber particles and the organic solvent into a reaction kettle, and adding an alkaline catalyst at the reflux temperature of the organic solvent to dissolve the silicon rubber particles to obtain a dissolved solution, wherein the dissolved solution contains crude organosilicon cyclic bodies;
a purification step: rearranging and rectifying the dissolved solution to obtain refined organosilicon ring bodies.
3. The process for recycling silicone rings from silicone rubber series substances as claimed in claim 2, wherein: the "pulverizing step" further comprises the steps of:
washing and drying the silicone rubber to obtain a clean material;
pulverizing and sieving the clean material to obtain the silicone rubber particles.
4. The process for recycling silicone rings from silicone rubber series substances as claimed in claim 2, wherein: the "purification step" further comprises the steps of:
adding water into the reaction kettle to obtain a mixed solution;
distilling the mixed solution under reduced pressure to separate the organic solvent;
and after the mixed solution is subjected to reduced pressure distillation, rearranging and rectifying the mixed solution to obtain the fine organosilicon ring body.
5. The process for recycling silicone rings from silicone rubber series substances as claimed in claim 4, wherein: the step of rearranging and rectifying the mixed solution to obtain the fine organosilicon ring bodies after the mixed solution is subjected to reduced pressure distillation further comprises the following steps of:
after the mixed solution is subjected to reduced pressure distillation, standing the mixed solution until the mixed solution is layered;
after the mixed solution is layered, obtaining an upper oil phase of the mixed solution, and rearranging and rectifying the upper oil phase to obtain the fine organosilicon ring body;
and obtaining a lower water phase of the mixed solution, and adsorbing and filtering the lower water phase to obtain a silicate aqueous solution.
6. The process for recycling silicone rings from silicone rubber series substances as claimed in claim 4, wherein: the pH value of the water is neutral or alkalescent.
7. The process for recycling silicone rings from silicone rubber series substances as claimed in claim 4, wherein: the mass ratio of the water to the dissolving solution is 0.4.
8. The process for recycling silicone rings of silicone rubber family substances according to any of claims 1 to 7, characterized in that: the mass ratio of the silicone rubber to the organic solvent is 30:100 to 100:30, of a nitrogen-containing gas;
the mass of the alkaline catalyst accounts for 3-15% of the mass of the silicon rubber.
9. The process for recovering silicone rings from a silicone rubber series according to any one of claims 1 to 7, wherein: the organic solvent comprises one or more of one-carbon alcohol, two-carbon alcohol, three-carbon alcohol, five-carbon alkanol, six-carbon alkanol, cyclane, dimethylamine, diethylamine, triethylamine, pentane, acetone and tetrahydrofuran.
10. The process for recycling silicone rings of silicone rubber family substances according to any of claims 1 to 7, characterized in that: the alkaline catalyst comprises one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, lithium methanol solution, sodium methanol solution, potassium methanol solution, lithium ethanol solution, sodium ethanol solution and potassium ethanol solution.
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