Preparation process of high-concentration high-stability methyl silicone oil emulsion
阅读说明：本技术 一种高浓高稳定甲基硅油乳液的制备工艺 (Preparation process of high-concentration high-stability methyl silicone oil emulsion ) 是由 郑敏 施斐 于 2019-10-31 设计创作，主要内容包括：本发明公开了一种高浓高稳定甲基硅油乳液的制备工艺,涉及硅油乳液相关技术领域,包括以下步骤：A：原料配制,B：原料混合,C：溶液水解,D：离心混合运动,E：脱底脱色反应,其中所述混合装置包括混合箱体,所述混合箱体的顶部固定连接有盖板,所述盖板的内顶壁固定连接有密封垫,所述混合箱体的底部固定连接有出料管道,所述出料管道的外表面固定安装有节流阀。本发明通过盖板方便了混合箱体的打开,方便混合箱体的内部进行清理,保证混合箱体的清洁,通过密封垫保证盖板的密封,通过出料管道方便了原料的排出,通过节流阀可以控制出料管道的排料速度,通过管道连接套方便了导料管道与出料管道的连接。(The invention discloses a preparation process of high-concentration and high-stability methyl silicone oil emulsion, which relates to the related technical field of silicone oil emulsion and comprises the following steps: a: preparing raw materials, B: raw material mixing, C: solution hydrolysis, D: centrifugal mixing motion, E: the decolourization reaction of taking off the end, wherein mixing arrangement is including mixing the box, the top fixedly connected with apron of mixing the box, the sealed pad of interior roof fixedly connected with of apron, the bottom fixedly connected with ejection of compact pipeline of mixing the box, the fixed surface of ejection of compact pipeline installs the choke valve. The invention facilitates the opening of the mixing box body through the cover plate, facilitates the cleaning of the interior of the mixing box body, ensures the cleaning of the mixing box body, ensures the sealing of the cover plate through the sealing gasket, facilitates the discharge of raw materials through the discharge pipeline, can control the discharge speed of the discharge pipeline through the throttle valve, and facilitates the connection of the material guide pipeline and the discharge pipeline through the pipeline connecting sleeve.)
1. A preparation process of high-concentration high-stability methyl silicone oil emulsion is characterized by comprising the following steps:
a: preparing raw materials: the methyl silicone oil consists of the following raw materials by mass percent of 70 percent, 4 percent of tallow amine polyethylene glycol ether, 1 percent of benzalkonium bromide and 25 percent of deionized water;
b: mixing raw materials: sequentially adding methyl silicone oil, tallow amine polyethenoxy ether, benzalkonium bromide and deionized water into a mixing device;
c: solution hydrolysis: the mixed solution flows to a hydrolysis reaction tower for hydrolysis reaction according to the volume flow of 500-600L/h, and only the water consumed by the hydrolysis reaction is replenished in the hydrolysis process at the hydrolysis temperature of 5-20 ℃;
d: centrifugal mixing movement: then carrying out bidirectional asymmetric centrifugal mixing motion on the solution after the hydrolysis reaction, setting the rotating speed at 2300rpm, and mixing for 60s while vacuumizing;
e: and (3) bottom removal and decoloration reaction: placing the solution obtained after filtration in a de-oligomerization kettle, heating to 110-;
wherein the mixing device comprises a mixing box body (1), the top of the mixing box body (1) is fixedly connected with a cover plate (2), the inner top wall of the cover plate (2) is fixedly connected with a sealing gasket (3), the bottom of the mixing box body (1) is fixedly connected with a discharge pipeline (4), a throttle valve (5) is fixedly arranged on the outer surface of the discharge pipeline (4), a pipeline connecting sleeve (6) is fixedly connected to the bottom of the discharge pipeline (4), the bottom of the pipeline connecting sleeve (6) is fixedly connected with a material guide pipeline (9), the outer surface of the material guiding pipeline (9) is fixedly connected with a sponge cushion (10), the outer surface of the spongy cushion (10) is fixedly connected with a frame sleeve body (11), both ends of the frame sleeve body (11) are fixedly connected with frame rods (12), and one end of each frame rod (12) is fixedly connected with a support column (13).
2. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
the viscosity of the simethicone in the step A is preferably 200000-700000 cs;
and D, the final vacuum degree in the step D reaches-0.08 to-0.09 MPao.
3. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
and C, performing hydrolysis twice, putting the obtained hydrolysate into a hydrolysate receiving kettle, and adding deionized water into the hydrolysate to perform secondary hydrolysis reaction.
4. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
and E, decoloring the primary methyl hydrogen-containing silicone oil and the activated carbon in a mass ratio of 1000:1, and filtering to obtain a finished methyl hydrogen-containing silicone oil product.
5. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
the top of the mixing box body (1) is attached to the bottom of the sealing gasket (3);
the bottom of the supporting column (13) is fixedly connected with a bottom plate (20).
6. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
one side of the top of the supporting column (13) is fixedly connected with a fixed frame plate (14);
the inner surface of the fixed frame plate (14) is fixedly connected with the outer surface of the mixing box body (1).
7. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
a feeding pipeline (16) is fixedly connected inside the cover plate (2);
the bottom of the feeding pipeline (16) is positioned inside the mixing box body (1).
8. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 1, characterized in that:
the top of the cover plate (2) is fixedly connected with a driving motor (15);
the bottom of the driving motor (15) is movably connected with a main shaft (17).
9. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 8, characterized in that:
the outer surface of the driving motor (15) is fixedly connected with a mounting sleeve (18);
the outer surface of the mounting sleeve (18) is fixedly connected with a plurality of stirring rods (19).
10. The preparation process of high-concentration high-stability methyl silicone oil emulsion according to claim 9, characterized in that:
the stirring rods (19) are arranged at equal intervals from top to bottom;
the mounting sleeve (18) and the stirring rod (19) are both positioned in the mixing box body (1).
Technical Field
The invention relates to the technical field of silicone oil emulsion, in particular to a preparation process of high-concentration and high-stability methyl silicone oil emulsion.
Background
The silicone oil is colorless, tasteless, nontoxic and non-irritant liquid, and has the characteristics of good chemical stability, heat resistance, cold resistance, weather resistance, lubricity, high refractive index, low surface tension and the like. The silicone oil emulsion prepared by emulsifying the silicone oil can be widely used for personal washing and caring articles, textiles and surface treatment. Methyl silicone oil emulsions generally require mixing of the raw materials during processing, however, existing mixing devices are not convenient to clean and the raw materials require external equipment for transportation.
Therefore, it is necessary to provide a preparation process of high-concentration and high-stability methyl silicone oil emulsion to solve the above problems.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation process of a high-concentration high-stability methyl silicone oil emulsion, which solves the problems that a mixing device is not convenient to clean and raw materials need to be transported by an external device.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation process of a high-concentration high-stability methyl silicone oil emulsion comprises the following steps:
a: preparing raw materials: the methyl silicone oil consists of the following raw materials by mass percent of 70 percent, 4 percent of tallow amine polyethylene glycol ether, 1 percent of benzalkonium bromide and 25 percent of deionized water;
b: mixing raw materials: sequentially adding methyl silicone oil, tallow amine polyethenoxy ether, benzalkonium bromide and deionized water into a mixing device;
c: solution hydrolysis: the mixed solution flows to a hydrolysis reaction tower for hydrolysis reaction according to the volume flow of 500-600L/h, and only the water consumed by the hydrolysis reaction is replenished in the hydrolysis process at the hydrolysis temperature of 5-20 ℃;
d: centrifugal mixing movement: then carrying out bidirectional asymmetric centrifugal mixing motion on the solution after the hydrolysis reaction, setting the rotating speed at 2300rpm, and mixing for 60s while vacuumizing;
e: and (3) bottom removal and decoloration reaction: placing the solution obtained after filtration in a de-oligomerization kettle, heating to 110-;
wherein mixing arrangement includes mixing box, mixing box's top fixedly connected with apron, the sealed pad of interior roof fixedly connected with of apron, mixing box's bottom fixedly connected with ejection of compact pipeline, ejection of compact pipeline's external surface fixed mounting has the choke valve, the bottom fixedly connected with pipeline adapter sleeve of ejection of compact pipeline, the bottom fixedly connected with guide pipe way of pipeline adapter sleeve, the external surface fixed connection of guide pipe way has the foam-rubber cushion, the external surface fixed connection of foam-rubber cushion has the frame set body, the equal fixedly connected with hack lever in both ends of the frame set body, the one end fixedly connected with support column of hack lever.
Optionally, the viscosity of the simethicone in the step A is preferably 200000-700000 cs;
and D, the final vacuum degree in the step D reaches-0.08 to-0.09 MPao.
Optionally, in the step C, hydrolysis is performed twice, the obtained hydrolysate is placed in a hydrolysate receiving kettle, and deionized water is added into the hydrolysate to perform a secondary hydrolysis reaction.
Optionally, in the step E, the mass ratio of the primary methyl hydrogen-containing silicone oil to the activated carbon is 1000:1, and the finished methyl hydrogen-containing silicone oil is obtained after activated carbon decolorization and filtration.
Optionally, the top of the mixing box body is attached to the bottom of the sealing gasket;
the bottom of the support column is fixedly connected with a bottom plate.
Optionally, a fixed frame plate is fixedly connected to one side of the top of the supporting column;
the inner surface of the fixed frame plate is fixedly connected with the outer surface of the mixing box body.
Optionally, a feeding pipeline is fixedly connected inside the cover plate;
the bottom of the feeding pipeline is positioned inside the mixing box body.
Optionally, the top of the cover plate is fixedly connected with a driving motor;
the bottom of the driving motor is movably connected with a main shaft.
Optionally, the outer surface of the driving motor is fixedly connected with an installation sleeve;
the outer surface of the mounting sleeve is fixedly connected with a plurality of stirring rods.
Optionally, a plurality of the stirring rods are arranged at equal intervals from top to bottom;
the mounting sleeve and the stirring rod are both positioned in the mixing box body.
(III) advantageous effects
The invention provides a preparation process of high-concentration and high-stability methyl silicone oil emulsion, which has the following beneficial effects:
(1) the invention facilitates the opening of the mixing box body through the cover plate, facilitates the cleaning of the interior of the mixing box body, ensures the cleaning of the mixing box body, ensures the sealing of the cover plate through the sealing gasket, prevents the raw materials from splashing, facilitates the discharge of the raw materials through the discharge pipeline, can control the discharge speed of the discharge pipeline through the throttle valve, and facilitates the connection of the material guide pipeline and the discharge pipeline through the pipeline connecting sleeve.
(2) The frame sleeve body can be used for facilitating the stabilization of the material guide pipeline and preventing the material guide pipeline from shaking, the frame sleeve body can be prevented from causing the abrasion of the material guide pipeline through the sponge mat, the frame rod and the support column can ensure the stability of the frame sleeve body, the transportation of mixed raw materials is facilitated through the material guide pipeline, and the transportation of the mixed raw materials using external raw materials is avoided.
Drawings
FIG. 1 is a schematic front view of the structure of the present invention;
FIG. 2 is a schematic view of the interior of the pipe coupling sleeve structure of the present invention;
FIG. 3 is a schematic view of the interior of the hybrid box structure of the present invention;
FIG. 4 is a schematic view of the connection of the frame sleeve body structure of the present invention.
In the figure: 1. a mixing box body; 2. a cover plate; 3. a gasket; 4. a discharge pipeline; 5. a throttle valve; 6. Connecting sleeves of pipelines; 7. sealing the ferrule; 8. a filter screen; 9. a material guide pipeline; 10. a sponge cushion; 11. a frame sleeve body; 12. a frame bar; 13. a support pillar; 14. fixing the frame plate; 15. a drive motor; 16. a feeding pipeline; 17. a main shaft; 18. installing a sleeve; 19. a stirring rod; 20. a base plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
In the present invention, unless otherwise expressly specified or limited, the terms "disposed," "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected or detachably connected; may be a mechanical connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The invention provides a technical scheme that:
a preparation process of a high-concentration high-stability methyl silicone oil emulsion comprises the following steps:
a: preparing raw materials: the methyl silicone oil consists of the following raw materials by mass percent of 70 percent, 4 percent of tallow amine polyethylene glycol ether, 1 percent of benzalkonium bromide and 25 percent of deionized water;
b: mixing raw materials: sequentially adding methyl silicone oil, tallow amine polyethenoxy ether, benzalkonium bromide and deionized water into a mixing device;
c: solution hydrolysis: the mixed solution flows to a hydrolysis reaction tower for hydrolysis reaction according to the volume flow of 500-600L/h, and only the water consumed by the hydrolysis reaction is replenished in the hydrolysis process at the hydrolysis temperature of 5-20 ℃;
d: centrifugal mixing movement: then carrying out bidirectional asymmetric centrifugal mixing motion on the solution after the hydrolysis reaction, setting the rotating speed at 2300rpm, and mixing for 60s while vacuumizing;
e: and (3) bottom removal and decoloration reaction: and (3) placing the filtered solution in a de-oligomerization kettle, heating to 110-140 ℃, controlling the pressure within-0.095 MPa, and controlling the de-oligomerization time to be more than 3 hours, wherein the methyl hydrogen-containing silicone oil primary product obtained after the reaction is placed in a decolorization kettle, and adding activated carbon for decolorization.
As an optional technical scheme of the invention:
the viscosity of the dimethyl silicone oil in the step A is preferably 200000-;
and D, the final vacuum degree reaches-0.08 to-0.09 MPao.
As an optional technical scheme of the invention:
and C, performing hydrolysis twice, putting the obtained hydrolysate into a hydrolysate receiving kettle, and adding deionized water into the hydrolysate to perform secondary hydrolysis reaction.
As an optional technical scheme of the invention:
and E, decoloring the primary methyl hydrogen-containing silicone oil and the activated carbon in a mass ratio of 1000:1, and filtering to obtain a finished methyl hydrogen-containing silicone oil product.
According to the drawings as shown in fig. 1-4, wherein the mixing device comprises a mixing box 1, a cover plate 2 is fixedly connected to the top of the mixing box 1, the opening of the mixing box 1 is facilitated through the cover plate 2, the cleaning of the interior of the mixing box 1 is facilitated, the cleanness of the mixing box 1 is ensured, a sealing gasket 3 is fixedly connected to the inner top wall of the cover plate 2, the sealing of the cover plate 2 is ensured through the sealing gasket 3, the raw materials are prevented from splashing, a discharging pipeline 4 is fixedly connected to the bottom of the mixing box 1, the discharging of the raw materials is facilitated through the discharging pipeline 4, a throttle valve 5 is fixedly installed on the outer surface of the discharging pipeline 4, the discharging speed of the discharging pipeline 4 can be controlled through the throttle valve 5, a pipeline connecting sleeve 6 is fixedly connected to the bottom of the discharging pipeline 4, a material guiding pipeline 9 is fixedly connected to the bottom of the pipeline, the transportation of the mixed raw materials is facilitated through the material guide pipeline 9, the outer surface of the transportation material guide pipeline 9 for avoiding the use of the external raw materials for the mixed raw materials is fixedly connected with the spongy cushion 10, the outer surface of the spongy cushion 10 is fixedly connected with the frame sleeve body 11, the stability of the material guide pipeline 9 can be facilitated through the frame sleeve body 11, the material guide pipeline 9 is prevented from shaking, the frame sleeve body 11 can be prevented from causing the abrasion of the material guide pipeline 9 through the spongy cushion 10, the two ends of the frame sleeve body 11 are both fixedly connected with the frame rods 12, one end of each frame rod 12 is fixedly connected with the support column 13, the stability of the frame sleeve body 11 can be ensured through the frame rods 12 and the support columns 13, the fixation of the mixing box body 1 can be ensured through the support columns 13 and the fixed frame plates, the mixing box body 1 is prevented from shaking or falling, the bottom of the support, the feeding pipeline 16 is fixedly connected inside the cover plate 2, the driving motor 15 is fixedly connected at the top of the cover plate 2, the main shaft 17 is movably connected at the bottom of the driving motor 15, the mounting sleeve 18 is fixedly connected at the outer surface of the driving motor 15, the stirring rods 19 are fixedly connected at the outer surface of the mounting sleeve 18, the main shaft 17 and the stirring rods 19 are conveniently driven by the driving motor 15 to rotate to mix raw materials, the mounting of the stirring rods 19 is facilitated by the mounting sleeve 18, the sealing ferrule 7 is fixedly connected at the lower part of the outer surface of the discharging pipeline 4, which facilitates the raw materials to be fed into the discharging pipeline 16, the leakage inside of the pipeline connecting sleeve 6 can be prevented by the sealing ferrule 7, the safety of the raw materials is increased, meanwhile, the safety of the pipeline connecting sleeve 6 can be ensured, the outer surface of the sealing ferrule 7 is fixedly connected with the inner surface of the pipeline connecting, the raw materials can be filtered through the filter screen 8, so that impurities in the raw materials can be prevented from affecting the quality of the methyl silicone oil emulsion.
The working principle is as follows: when in work, raw materials are added into the
It is noted that in the present disclosure, unless otherwise explicitly specified or limited, a first feature "on" or "under" a second feature may be directly contacted with the first and second features, or indirectly contacted with the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
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