CN113636564A - Green preparation method of white carbon black - Google Patents
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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Abstract
The invention relates to a green preparation method of white carbon black, which comprises the following steps: (1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; (2) and (2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain the white carbon black. According to the invention, the process of preparing the white carbon black by the sol-gel method is adjusted, the problem of insufficient fire resistance of the fire-resistant silicon rubber is solved in a targeted manner by introducing the auxiliary agent, homogenizing treatment and protective atmosphere, the pore diameter and the specific surface of the white carbon black are reasonably regulated and controlled, and the white carbon black can further play a role in the fire-resistant silicon rubber.
Description
Technical Field
The invention relates to the field of white carbon black, and particularly relates to a green preparation method of white carbon black.
Background
At present, the white carbon black has good physical and chemical properties, and is widely applied to various industries, such as refractory materials to improve the refractory performance of the refractory materials.
For example, CN102850805A discloses a ceramic fire-resistant silicone rubber, a preparation method thereof and an application thereof in electric wires and cables, wherein the rubber comprises 100 parts of methyl vinyl silicone rubber, 30-80 parts of white carbon black, 9-40 parts of alumina, 1.5-8 parts of a structure control agent, 3-5 parts of a sintering additive, 0.25-1.5 parts of a surface treatment agent and 0.5-2 parts of a cross-linking agent. The preparation method comprises the following steps: mixing raw methyl vinyl silicone rubber with a rubber covered roll, sequentially adding white carbon black, alumina, a surface treating agent, a structure control agent, a sintering additive and a crosslinking agent, uniformly mixing, and remilling the parked rubber to recover plasticity to obtain the ceramic fire-resistant silicone rubber. The refractory silicon rubber material has the characteristics of compact ceramic body, stable structure, stable refractory performance, good insulating performance and the like.
CN110862687A discloses a preparation method of a ceramic fire-resistant silicone rubber composite material, which comprises the following steps: s1, preparing the following raw materials in parts by weight: 50-300 parts of vitrified powder, 80-120 parts of silicone rubber, 5-100 parts of a flame retardant, 5-50 parts of white carbon black, 1-50 parts of a cosolvent, 1-30 parts of a catalyst, 1-10 parts of silicone oil, 1-4 parts of a vulcanizing agent, 0.1-5 parts of a coupling agent and 0.1-1 part of a platinum complex; s2, adding the porcelain powder and the coupling agent in parts by weight into a mixer, mixing for 10-14 min at the speed of 1600-2000 r/min, adding the flame retardant, and continuously mixing for 10-14 min at the speed of 1600-2000 r/min to obtain a mixture A. The fireproof cable can be applied to high, medium and low voltage fireproof electric wires and cables, flexible fireproof cables, fireproof electric power and control cables, and is worthy of popularization.
However, the fire-resistant silicone rubber obtained at present still has the problems of low fire-resistant temperature, short fire-resistant time and the like.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a green preparation method of white carbon black, so as to solve the problems of low fire resistance temperature and short fire resistance time when nano silicon dioxide is used for fire-resistant silicone rubber. When the obtained nano silicon dioxide is used as an auxiliary material of the fire-resistant silicon rubber, the mechanical property of the fire-resistant silicon rubber can be improved, and the service life of the fire-resistant silicon rubber is further prolonged.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a green preparation method of white carbon black, which comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment;
(2) and (2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain the white carbon black.
According to the invention, the process of preparing the white carbon black by the sol-gel method is adjusted, the problem of insufficient fire resistance of the fire-resistant silicon rubber is solved in a targeted manner by introducing the auxiliary agent, homogenizing treatment and protective atmosphere, the pore diameter and the specific surface of the white carbon black are reasonably regulated and controlled, and the white carbon black can further play a role in the fire-resistant silicon rubber.
As a preferred embodiment of the present invention, the volume ratio of the vinyltrimethoxysilane to the carbonate solution in step (1) is 1:1.5 to 2, and examples thereof include 1:1.5, 1:1.52, 1:1.54, 1:1.56, 1:1.58, 1:1.6, 1:1.62, 1:1.64, 1:1.66, 1:1.68, 1:1.7, 1:1.72, 1:1.74, 1:1.76, 1:1.78, 1:1.8, 1:1.82, 1:1.84, 1:1.86, 1:1.88, 1:1.9, 1:1.92, 1:1.94, 1:1.96, 1:1.98 and 1:2, but are not limited thereto, and other combinations not specifically recited therein are also applicable.
In a preferred embodiment of the present invention, the mass concentration of the auxiliary in step (1) is 20 to 35%, and may be, for example, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, or 35%, but is not limited to the above-mentioned values, and other combinations not shown in the above-mentioned range are also applicable.
As a preferable technical scheme of the invention, the auxiliary agent in the step (1) comprises carbonate solution and/or bicarbonate solution.
Preferably, the carbonate solution comprises a sodium carbonate solution and/or a potassium carbonate solution.
Preferably, the bicarbonate solution comprises a sodium bicarbonate solution and/or a potassium bicarbonate solution.
As a preferred embodiment of the present invention, the pressure of the homogenization treatment in the step (1) is 20 to 40MPa, and may be, for example, 20MPa, 21MPa, 22MPa, 23MPa, 24MPa, 25MPa, 26MPa, 27MPa, 28MPa, 29MPa, 30MPa, 31MPa, 32MPa, 33MPa, 34MPa, 35MPa, 36MPa, 37MPa, 38MPa, 39MPa or 40MPa, but the present invention is not limited to the values listed above, and other combinations not listed above within the range are also applicable.
Preferably, the temperature of the homogenization treatment in step (1) is 100-.
Preferably, the time for the homogenization treatment in step (1) is 1 to 2 hours, and for example, 1 hour, 1.1 hour, 1.2 hours, 1.3 hours, 1.4 hours, 1.5 hours, 1.6 hours, 1.7 hours, 1.8 hours, 1.9 hours, or 2 hours, etc., but not limited to the values listed, and other combinations not listed within this range are also applicable.
In a preferred embodiment of the present invention, the mass ratio of the material to the alcohol in the step (2) is 1 (0.2 to 0.7), and examples thereof include 1:0.2, 1:0.22, 1:0.24, 1:0.26, 1:0.28, 1:0.3, 1:0.32, 1:0.34, 1:0.36, 1:0.38, 1:0.4, 1:0.42, 1:0.44, 1:0.46, 1:0.48, 1:0.5, 1:0.52, 1:0.54, 1:0.56, 1:0.58, 1:0.6, 1:0.62, 1:0.64, 1:0.66, 1:0.68 and 1:0.7, but not limited thereto, and other combinations not specifically recited in this range are also applicable.
As a preferable technical scheme of the invention, the protective atmosphere in the step (2) comprises ammonia gas.
Preferably, the volume percentage of ammonia gas in the protective atmosphere in step (2) is 40-50%, for example, 40%, 40.5%, 41%, 41.5%, 42%, 42.5%, 43%, 43.5%, 44%, 44.5%, 45%, 45.5%, 46%, 46.5%, 47%, 47.5%, 48%, 48.5%, 49%, 49.5% or 50%, etc., but not limited to the recited values, and other combinations not recited in this range are also applicable.
As a preferred embodiment of the present invention, the temperature of the reaction in the step (2) is 75 to 90 ℃ and may be, for example, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃ or 90 ℃ or the like, but is not limited to the values listed, and other combinations not listed within the range are also applicable.
Preferably, the reaction time in step (2) is 20-40min, such as 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min or 40min, but not limited to the values listed, and other combinations not listed in this range are also applicable.
As a preferred embodiment of the present invention, the temperature of aging in the step (2) is 30 to 50 ℃ and may be, for example, 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃ or 50 ℃ or the like, but is not limited to the values listed, and other combinations not listed in this range are also applicable.
Preferably, the aging time in step (2) is 3 to 4 hours, such as 3 hours, 3.1 hours, 3.2 hours, 3.3 hours, 3.4 hours, 3.5 hours, 3.6 hours, 3.7 hours, 3.8 hours, 3.9 hours, or 4 hours, but not limited to the recited values, and other combinations not recited in this range are also applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1 (1.5-2); the mass concentration of the auxiliary agent is 20-35%; the auxiliary agent comprises a carbonate solution and/or a bicarbonate solution; the carbonate solution comprises a sodium carbonate solution and/or a potassium carbonate solution; the bicarbonate solution comprises sodium bicarbonate solution and/or potassium bicarbonate solution; the pressure of the homogenization treatment is 20-40 MPa; the temperature of the homogenization treatment is 100-150 ℃; the homogenizing treatment time is 1-2 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1 (0.2-0.7); the protective atmosphere comprises ammonia; the volume percentage of ammonia in the protective atmosphere is 40-50%; the reaction temperature is 75-90 ℃; the reaction time is 20-40 min; the aging temperature is 30-50 ℃; the aging time is 3-4 h.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the invention, the process of preparing the white carbon black by the sol-gel method is adjusted, the problem of insufficient fire resistance of the fire-resistant silicon rubber is solved in a targeted manner by introducing the auxiliary agent, homogenizing treatment and protective atmosphere, the pore diameter and the specific surface of the white carbon black are reasonably regulated and controlled, and the white carbon black can further play a role in the fire-resistant silicon rubber.
(2) According to the invention, the pore size distribution and the specific surface index in the white carbon black forming process are controlled by introducing the auxiliary agent and the protective atmosphere, so that the obtained white carbon black has excellent pore size distribution composition, the formation of closed pores in the obtained white carbon black product is reduced, and the release of the performance of the white carbon black in silicon rubber is facilitated.
(3) According to the preparation method provided by the invention, the prepared white carbon black has the particle size of 12-20nm and the BET specific surface area of more than or equal to 248.33m2And/g, the fire resistance and the mechanical property of the fire-resistant rubber can be obviously improved by adding the flame-resistant rubber into the fire-resistant rubber.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a green preparation method of white carbon black, which comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1: 1.7; the mass concentration of the auxiliary agent is 23%; the auxiliary agent is a sodium carbonate solution; the pressure of the homogenization treatment is 25 MPa; the temperature of the homogenization treatment is 120 ℃; the homogenizing treatment time is 1.7 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1: 0.5; the protective atmosphere comprises ammonia; the volume percentage of ammonia in the protective atmosphere is 47%; the temperature of the reaction was 87 ℃; the reaction time is 37 min; the temperature of the aging is 33 ℃; the aging time was 3.7 h.
The performance parameters of the obtained white carbon black are detailed in table 1.
Example 2
The embodiment provides a green preparation method of white carbon black, which comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1: 1.5; the mass concentration of the auxiliary agent is 35%; the auxiliary agent is potassium bicarbonate solution; the pressure of the homogenization treatment is 40 MPa; the temperature of the homogenization treatment is 100 ℃; the homogenizing treatment time is 1 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1: 0.7; the protective atmosphere comprises ammonia; the volume percentage of ammonia in the protective atmosphere is 50%; the temperature of the reaction is 75 ℃; the reaction time is 40 min; the temperature of the aging is 50 ℃; the aging time is 3 h.
The performance parameters of the obtained white carbon black are detailed in table 1.
Example 3
The embodiment provides a green preparation method of white carbon black, which comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1: 2; the mass concentration of the auxiliary agent is 20%; the auxiliary agent is potassium carbonate solution; the pressure of the homogenization treatment is 20 MPa; the temperature of the homogenization treatment is 150 ℃; the homogenization treatment time is 2 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1: 0.2; the protective atmosphere comprises ammonia; the volume percentage content of ammonia in the protective atmosphere is 40%; the temperature of the reaction is 90 ℃; the reaction time is 20 min; the temperature of the aging is 30 ℃; the aging time is 4 h.
The performance parameters of the obtained white carbon black are detailed in table 1.
Example 4
The embodiment provides a green preparation method of white carbon black, which comprises the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1: 1.8; the mass concentration of the auxiliary agent is 31 percent; the auxiliary agent is a mixed solution of sodium carbonate and potassium bicarbonate, and the molar ratio is 1: 1; the pressure of the homogenization treatment is 32 MPa; the temperature of the homogenization treatment is 137 ℃; the homogenizing treatment time is 1.4 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1: 0.3; the protective atmosphere comprises ammonia; the volume percentage of ammonia in the protective atmosphere is 44%; the temperature of the reaction is 80 ℃; the reaction time is 28 min; the aging temperature is 41 ℃; the aging time was 3.4 h.
The performance parameters of the obtained white carbon black are detailed in table 1.
Comparative example 1
The only difference from example 1 is that the auxiliary agent is replaced by an equal amount of water. The performance parameters of the obtained white carbon black are detailed in table 1.
Comparative example 2
The only difference from example 1 is that the subsequent operation was carried out without homogenizing after mixing, and directly mixing with alcohol. The performance parameters of the obtained white carbon black are detailed in table 1.
Comparative example 3
The only difference from example 1 is that the reaction was carried out under an argon atmosphere after mixing step (2) with alcohol. The performance parameters of the obtained white carbon black are detailed in table 1.
Comparative example 4
The only difference from example 1 is that the auxiliary in step (1) is replaced by an equivalent amount of ammonia water of equivalent concentration. The performance parameters of the obtained white carbon black are detailed in table 1.
Comparative example 5
The only difference from example 1 is that the mass ratio of the feed to the alcohol in step (2) is 1: 2. The performance parameters of the obtained white carbon black are detailed in table 1.
The white carbon black obtained in example 1 and comparative example 1 is used as an admixture to prepare fire-resistant silicone rubber.
The method A comprises the following steps: prepared according to the method of example 1 in CN 110643183A; the corresponding tensile strength in the publication is 11.7MPa, the maximum tolerance temperature is 500 ℃, and the fire-resistant time is 30-60 min;
the method B comprises the following steps: prepared according to the method of example 1 in CN 103665881A; the corresponding tensile strength in the publication is 9.3MPa, the fire resistance time is 90min, and the maximum fire resistance temperature is 600 ℃ through the detection of the inventor;
the method C comprises the following steps: prepared according to the method of example 1 in CN 112625447A; the corresponding tensile strength in the publication is 5.6MPa, and the maximum fire-resistant temperature is 550 ℃ and the fire-resistant time is 60min according to the detection of the inventor.
The performance indexes of the silicone rubber obtained by the preparation method are detailed in table 2.
TABLE 1
TABLE 2
According to the results of the above examples and comparative examples, in the invention, the process of preparing the white carbon black by the sol-gel method is adjusted, the problem of insufficient fire resistance of the fire-resistant silicone rubber is solved by introducing the auxiliary agent, homogenizing treatment and protective atmosphere, the pore diameter and specific surface of the white carbon black are reasonably regulated and controlled, and the white carbon black can further play a role in the fire-resistant silicone rubber.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The green preparation method of the white carbon black is characterized by comprising the following steps:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment;
(2) and (2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain the white carbon black.
2. The method according to claim 1, wherein the volume ratio of the vinyltrimethoxysilane to the carbonate solution in the step (1) is 1 (1.5-2).
3. The production method according to claim 1 or 2, wherein the mass concentration of the auxiliary in the step (1) is 20 to 35%.
4. The method according to any one of claims 1 to 3, wherein the auxiliary in step (1) comprises a carbonate solution and/or a bicarbonate solution;
preferably, the carbonate solution comprises a sodium carbonate solution and/or a potassium carbonate solution;
preferably, the bicarbonate solution comprises a sodium bicarbonate solution and/or a potassium bicarbonate solution.
5. The production method according to any one of claims 1 to 4, wherein the pressure of the homogenization treatment in the step (1) is 20 to 40 MPa;
preferably, the temperature of the homogenization treatment in the step (1) is 100-150 ℃;
preferably, the time of the homogenization treatment in the step (1) is 1-2 h.
6. The production method according to any one of claims 1 to 5, wherein the mass ratio of the material to the alcohol in the step (2) is 1 (0.2 to 0.7).
7. The method according to any one of claims 1 to 6, wherein the protective atmosphere in step (2) comprises ammonia gas;
preferably, the volume percentage of the ammonia gas in the protective atmosphere in the step (2) is 40-50%.
8. The method according to any one of claims 1 to 7, wherein the temperature of the reaction in the step (2) is 75 to 90 ℃;
preferably, the reaction time of the step (2) is 20-40 min.
9. The production method according to any one of claims 1 to 8, wherein the temperature of aging in step (2) is 30 to 50 ℃;
preferably, the aging time of step (2) is 3-4 h.
10. The method of any one of claims 1-9, comprising:
(1) mixing vinyl trivalent oxysilane and an auxiliary agent, and then carrying out homogenization treatment; the volume ratio of the vinyl trivalent oxylsilane to the carbonate solution is 1 (1.5-2); the mass concentration of the auxiliary agent is 20-35%; the auxiliary agent comprises a carbonate solution and/or a bicarbonate solution; the carbonate solution comprises a sodium carbonate solution and/or a potassium carbonate solution; the bicarbonate solution comprises sodium bicarbonate solution and/or potassium bicarbonate solution; the pressure of the homogenization treatment is 20-40 MPa; the temperature of the homogenization treatment is 100-150 ℃; the homogenizing treatment time is 1-2 h;
(2) mixing the material obtained by the homogenization treatment in the step (1) with alcohol, reacting in a protective atmosphere, and then sequentially aging and carrying out solid-liquid separation on the material obtained by the reaction to obtain white carbon black; the mass ratio of the materials to the alcohol is 1 (0.2-0.7); the protective atmosphere comprises ammonia; the volume percentage of ammonia in the protective atmosphere is 40-50%; the reaction temperature is 75-90 ℃; the reaction time is 20-40 min; the aging temperature is 30-50 ℃; the aging time is 3-4 h.
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