CN115364793A - Preparation method and device of fatty secondary alcohol polyoxyethylene ether - Google Patents
Preparation method and device of fatty secondary alcohol polyoxyethylene ether Download PDFInfo
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- CN115364793A CN115364793A CN202210146546.2A CN202210146546A CN115364793A CN 115364793 A CN115364793 A CN 115364793A CN 202210146546 A CN202210146546 A CN 202210146546A CN 115364793 A CN115364793 A CN 115364793A
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- secondary alcohol
- polyoxyethylene ether
- alcohol polyoxyethylene
- mixing tank
- pipe
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- 229920000056 polyoxyethylene ether Polymers 0.000 title claims abstract description 63
- 229940051841 polyoxyethylene ether Drugs 0.000 title claims abstract description 62
- 150000003333 secondary alcohols Chemical class 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 238000002156 mixing Methods 0.000 claims abstract description 46
- 238000005086 pumping Methods 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 239000012043 crude product Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000009471 action Effects 0.000 claims abstract description 8
- 239000003377 acid catalyst Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- 239000003463 adsorbent Substances 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 17
- -1 aliphatic secondary alcohol Chemical class 0.000 claims description 13
- 239000011229 interlayer Substances 0.000 claims description 13
- 230000000712 assembly Effects 0.000 claims description 12
- 238000000429 assembly Methods 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- 241000220317 Rosa Species 0.000 claims 2
- 239000008213 purified water Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical group C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000002761 deinking Substances 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000012994 industrial processing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical group OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000004563 wettable powder Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2696—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the process or apparatus used
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical industry, and particularly discloses a preparation method and a device of fatty secondary alcohol polyoxyethylene ether; the method comprises the following steps: s1, carrying out contact reaction on secondary alcohol and ethylene oxide under the action of an acid catalyst to obtain a crude product of fatty secondary alcohol polyoxyethylene ether; s2, transferring the crude product of the fatty secondary alcohol polyoxyethylene ether into a tank, adding water, stirring, and then standing for layering; s3, after the mixed liquid is kept stand and layered, pumping the oil phase into a filter for adsorption, impurity removal and decoloration; s4, pumping the liquid after impurity removal and decoloration into a rectifying still for rectification to obtain the fatty secondary alcohol polyoxyethylene ether; the preparation method disclosed by the invention comprises the steps of mixing and stirring the prepared crude product of the fatty secondary alcohol polyoxyethylene ether with purified water, standing for layering, then sending the layered oil phase into a filter for adsorption and impurity removal by activated carbon, decoloring, and finally rectifying in a low-temperature environment, so that the prepared fatty secondary alcohol polyoxyethylene ether has higher purity and wider application range.
Description
Technical Field
The invention relates to the technical field of preparation of fatty secondary alcohol polyoxyethylene ether, and particularly discloses a preparation method and a device of fatty secondary alcohol polyoxyethylene ether.
Background
The fatty secondary alcohol polyoxyethylene ether is an excellent penetrating, emulsifying, wetting and cleaning agent, has good biodegradability and environmental friendliness when being used as various liquid agents, and has various performances close to TX series and superior to linear AEO series; meanwhile, the water-soluble polymer can be compounded with other various anionic, nonionic and cationic surfactants for use, has a superior synergistic effect, can greatly reduce the use and consumption of the auxiliary agent, and achieves good cost performance; the efficacy of thickeners for paints and the washability of solvent-based systems can be improved. The method has wide application in textile printing and dyeing refining bleaching, paint emulsifying agents, papermaking deinking agents, pesticide and fertilizer wettable powder emulsifying agents, dry cleaning agents, textile treatment and oil field exploitation.
The prior preparation process of the fatty secondary alcohol polyoxyethylene ether is obtained by reacting secondary alcohol and ethylene oxide under the action of a catalyst, for example, the invention patent with the application number of 2018101842857 discloses a preparation method of the fatty secondary alcohol polyoxyethylene ether, which at least comprises the following steps: carrying out contact reaction on secondary alcohol, ethylene oxide and an acidic catalyst to obtain fatty secondary alcohol polyoxyethylene ether; however, the purity of the fatty secondary alcohol polyoxyethylene ether prepared by the process is low, so that the application field of the fatty secondary alcohol polyoxyethylene ether is greatly limited. Although the prior patent also discloses a method for purifying the prepared fatty secondary alcohol polyoxyethylene ether, the specific steps comprise adding the obtained fatty secondary alcohol polyoxyethylene ether into an alkaline solution, then adding an extracting agent, starting stirring, and obtaining the fatty secondary alcohol polyoxyethylene ether after standing, liquid separation, water phase removal and rectification in sequence. However, the method still cannot remove impurities, pigments and the like in the fatty secondary alcohol polyoxyethylene ether only by standing, separating and dehydrating and rectifying, and meanwhile, because of the limitation of the existing preparation device, the whole steps can only be carried out in a laboratory step mode when the fatty secondary alcohol polyoxyethylene ether is subjected to standing, separating and dehydrating, and chemical industrial processing cannot be realized. Therefore, the application provides a method and a device for preparing the fatty secondary alcohol polyoxyethylene ether, which can solve the technical problems, aiming at the defects that the existing preparation process of the fatty secondary alcohol polyoxyethylene ether can not prepare high-purity fatty secondary alcohol polyoxyethylene ether and can not realize industrial treatment due to the limitation of the device.
Disclosure of Invention
The invention aims to design a method and a device for preparing fatty secondary alcohol polyoxyethylene ether, which can solve the technical problems, aiming at the defects that the prior preparation process of fatty secondary alcohol polyoxyethylene ether can not prepare high-purity fatty secondary alcohol polyoxyethylene ether and can not realize industrial treatment due to the limitation of the device.
The invention is realized by the following technical scheme:
a preparation method of fatty secondary alcohol polyoxyethylene ether comprises the following steps:
s1: carrying out contact reaction on secondary alcohol and ethylene oxide under the action of an acid catalyst to obtain a crude product of the fatty secondary alcohol polyoxyethylene ether;
s2: transferring the crude product of the fatty secondary alcohol polyoxyethylene ether into a tank, adding water, stirring, and then standing for layering;
s3: after the mixed liquid is kept stand and layered, pumping the oil phase into a filter for adsorption, impurity removal and decoloration;
s4: and pumping the liquid after impurity removal and decoloration into a rectifying still for rectification to obtain the fatty secondary alcohol polyoxyethylene ether.
Preferably, the acidic catalyst in step 1 is H 2 SO 4 、HClO 4 And anhydrous stannic chloride or aluminum chloride.
Preferably, the rectification temperature in the step 4 is controlled within the range of 40-48 ℃.
A preparation device used in the preparation method of the fatty secondary alcohol polyoxyethylene ether is equipment in steps and comprises a mixing tank body, a filter and a control cabinet, wherein the upper surface of the mixing tank body is provided with a first liquid injection pipe and a second liquid injection pipe, a stirring rack is arranged in the mixing tank body, the upper end of the mixing tank body is provided with a stirring motor for driving the stirring rack, the lower end of the mixing tank body is connected with a liquid discharge pipe, and a first manual valve is arranged on the liquid discharge pipe;
the side surface of the mixing tank body close to the filter is provided with a vertical strip-shaped opening, a telescopic interlayer is hermetically connected in the strip-shaped opening, a moving block is fixedly connected in the telescopic interlayer, an oil pumping pipe penetrates through the moving block, the inner end of the oil pumping pipe is communicated with the inner cavity of the mixing tank body, the outer end of the oil pumping pipe is provided with a first electromagnetic valve, the side surface of the moving block is connected with a lug, the lug is provided with a threaded hole, the outer surface of the mixing tank body above and below the lug is fixedly connected with rotating seats, a vertically arranged screw rod is connected between the two rotating seats and matched with the threaded hole on the lug, the outer surface of the mixing tank body is also provided with a screw rod motor connected with the end part of the screw rod, and the mixing tank body at the strip-shaped side opening is provided with a vertical strip-shaped glass observation window;
the filter comprises a filter box, at least two filter assemblies are arranged in the filter box, a liquid pump is fixed on the side surface of the filter box close to the mixing tank body, the liquid inlet end of the liquid pump is connected with the outer end of an oil pumping pipe through a hose, the liquid outlet end of the liquid pump is connected with an oil conveying pipe, the upper end of the oil conveying pipe is connected with a plurality of branch pipes, second electromagnetic valves are arranged on the branch pipes, and the branch pipes are connected with the corresponding filter assemblies;
the filter assembly comprises a cylinder vertically and fixedly arranged in the filter box, the lower end of the cylinder is connected with a slag discharge pipe extending out of the filter box, a second manual valve is arranged on the slag discharge pipe, a hollow rotating pipe is coaxially and rotatably connected in the cylinder, a driven gear is arranged at the upper end of the hollow rotating pipe extending out of the cylinder, a driving motor is arranged on the upper surface of the filter box, the lower end of an output shaft of the driving motor extending into the filter box is connected with a driving gear, the driving gear and the driven gear are meshed, spiral blades are arranged on the outer surface of the hollow rotating pipe positioned in the cylinder, a large number of oil outlet holes are formed in the upper end of the cylinder, a bearing rotatably connected with the hollow rotating pipe is further arranged on the upper surface of the filter box, the top end of the hollow rotating pipe extending out of the filter box is connected with a sealed rotating connecting piece, and the sealed rotating connecting piece is rotatably connected with the lower end of the branch pipe;
the upper surface of the filter box is also fixedly provided with an adsorbent storage hopper corresponding to each filter assembly, the lower end of the adsorbent storage hopper is connected with a material guide channel, the lower end of the material guide channel is communicated with the upper end of the cylinder, the lower end of the filter box is provided with a material discharge pipe, and a third manual valve is arranged on the material discharge pipe.
As a further arrangement of the scheme, a plurality of supporting legs are uniformly connected to the circumferential direction of the lower end of the mixing tank body.
As the further setting of above-mentioned scheme, the agitator includes the dwang that is connected with agitator motor output shaft, be connected with a large amount of stirring rods on the dwang.
As a further arrangement of the scheme, the telescopic interlayer is made of rubber materials or plastic materials, and the moving block is fixedly and hermetically connected with the telescopic interlayer.
As a further arrangement of the scheme, 2-5 filter assemblies are arranged in the filter box.
As a further arrangement of the scheme, the length of the strip-shaped glass observation window is larger than that of the strip-shaped opening, and the strip-shaped glass observation window and the strip-shaped opening are both arranged at the height position of 1/3-2/3 of the mixing tank body.
As a further arrangement of the above scheme, the adsorbent storage hopper is filled with a large amount of activated carbon adsorbent.
Compared with the prior art, the invention has the beneficial effects that:
1) The preparation method of the fatty secondary alcohol polyoxyethylene ether disclosed by the invention comprises the steps of mixing and stirring the prepared crude fatty secondary alcohol polyoxyethylene ether with purified water, standing for layering, then sending the layered oil phase into a filter for activated carbon adsorption, impurity removal and decoloration, and finally rectifying in a low-temperature environment, so that the prepared fatty secondary alcohol polyoxyethylene ether has higher purity and wider application range.
2) The preparation device disclosed by the invention is improved by depending on the preparation method, after oil is kept standing and layered, the positive and negative rotation of the screw rod can be controlled by penetrating through the position of an oil boundary layer, so that the oil pumping pipe is adjusted to the lower end of an oil phase for extraction, the layered oil phase is convenient to extract, the height of the oil interface is convenient to adjust, the preparation device is suitable for separation after different crude products and water are mixed, the structural design is novel, the use is convenient, and the industrial purification preparation of the fatty secondary alcohol polyoxyethylene ether is effectively realized.
3) The preparation device disclosed by the invention has the advantages that the filter is internally provided with the plurality of filter assemblies which are arranged one by one, when the internal adsorbent needs to be replaced after long-time filtration, the invalid adsorbent can be automatically discharged through the design of the special structure of the filter assemblies, and then the new adsorbent is automatically filled in, so that the automation degree of the whole equipment is high, and the whole processes of filtering, impurity removal and decoloration cannot be interrupted even in the process of replacing the adsorbent, and the preparation efficiency of the high-purity aliphatic secondary alcohol polyoxyethylene ether is greatly improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of the manufacturing process of the present invention;
FIG. 2 is a schematic view of a first-angle perspective structure of a manufacturing apparatus according to the present invention;
FIG. 3 is a schematic view of a second angular perspective structure of the manufacturing apparatus of the present invention;
FIG. 4 is a schematic perspective view of a mixing tank according to the present invention;
FIG. 5 is a schematic view of the internal plan structure of the mixing tank of the present invention;
FIG. 6 is an enlarged view of the structure at A in FIG. 3 according to the present invention;
FIG. 7 is a schematic view of a three-dimensional structure of a telescopic interlayer, a moving block, an oil pumping pipe and the like in the invention;
FIG. 8 is a schematic view showing the inner plan structure of the filter according to the present invention;
FIG. 9 is a schematic perspective view of a filter assembly, an adsorbent storage hopper, etc. according to the present invention;
FIG. 10 is a perspective half sectional view of the filter assembly of the present invention;
FIG. 11 is a schematic perspective view of a hollow rotating tube and a spiral blade according to the present invention.
Wherein:
100-a mixing tank body, 101-a first liquid injection pipe, 102-a second liquid injection pipe, 103-a stirring frame, 104-a stirring motor, 105-a liquid discharge pipe, 106-a first manual valve, 107-a strip-shaped opening, 108-a telescopic interlayer, 109-a moving block, 110-an oil pumping pipe, 111-a first electromagnetic valve, 112-a bump, 113-a rotating seat, 114-a screw rod, 115-a screw rod motor, 116-a strip-shaped glass observation window and 117-supporting legs;
200-filter, 201-filter box, 202-filter component, 2021-cylinder, 2022-slag discharge pipe, 2023-second manual valve, 2024-hollow rotating pipe, 2025-driven gear, 2026-driving motor, 2027-driving gear, 2028-helical blade, 2029-oil outlet, 2030-sealing rotating connecting piece, 204-adsorbent storage hopper, 205-guide channel, 206-discharge pipe, 207-third manual valve;
300-control cabinet.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments in the present application without making any creative effort shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the foregoing drawings are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used.
Moreover, the terms "mounted," "disposed," "connected," "coupled," and "coupled" are to be construed broadly. For example, it may be a fixed connection, a removable connection, or a unitary construction; can be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements or components. The specific meanings of the above terms in the present invention can be understood by those of ordinary skill in the art according to specific situations.
It should be noted that, in the present application, the embodiments and features of the embodiments may be combined with each other without conflict. The present application will be described in detail with reference to the accompanying drawings 1 to 11, in conjunction with the embodiments.
Example 1:
embodiment 1 discloses a preparation method of fatty secondary alcohol polyoxyethylene ether, which comprises the following steps:
s1: and (3) carrying out contact reaction on secondary alcohol and ethylene oxide under the action of an acid catalyst to obtain a crude product of the fatty secondary alcohol polyoxyethylene ether, wherein the carbon atom number of the secondary alcohol is 14, and the selected acid catalyst is HClO4.
S2: and transferring the crude product of the aliphatic secondary alcohol polyoxyethylene ether into a tank, adding water until the volume of the crude product is about 80% of that of the tank, stirring, and then standing for layering.
S3: and after the mixed liquid is kept stand and layered, pumping the oil phase into a filter, and adsorbing, removing impurities and decoloring by using an activated carbon adsorbent in the filter.
S4: pumping the liquid after impurity removal and decoloration into a rectifying still, then rectifying at the temperature of 45 ℃, and obtaining the fatty secondary alcohol polyoxyethylene ether after rectification.
Example 2:
embodiment 2 discloses a preparation method of fatty secondary alcohol polyoxyethylene ether, which comprises the following steps:
s1: and (2) carrying out contact reaction on secondary alcohol and ethylene oxide under the action of an acid catalyst to obtain a crude product of the aliphatic secondary alcohol polyoxyethylene ether, wherein the carbon atom number of the secondary alcohol is 14, and the selected acid catalyst is aluminum chloride.
S2: and transferring the crude product of the aliphatic secondary alcohol polyoxyethylene ether into a tank, adding water until the volume of the crude product is about 75% of that of the tank, stirring, and then standing for layering.
S3: and after the mixed liquid is kept stand and layered, pumping the oil phase into a filter, and adsorbing, removing impurities and decoloring by using an activated carbon adsorbent in the filter.
S4: pumping the liquid after impurity removal and decoloration into a rectifying still, then rectifying at the temperature of 48 ℃, and obtaining the fatty secondary alcohol polyoxyethylene ether after rectification.
In summary, in the preparation methods of the secondary aliphatic alcohol polyoxyethylene ethers disclosed in embodiments 1 and 2, a secondary alcohol and ethylene oxide are reacted by a conventional preparation method to prepare a crude secondary aliphatic alcohol polyoxyethylene ether product, then the crude product is mixed with water, stood for layering, an oil phase is fed into a filter to be adsorbed by activated carbon for impurity removal and decolorization, and then rectification is performed, so that the purity of the prepared secondary aliphatic alcohol polyoxyethylene ether is effectively ensured, and the prepared secondary aliphatic alcohol polyoxyethylene ether has a wider application range.
Example 3:
example 3 discloses a preparation apparatus used in examples 1 and 2, and referring to fig. 2 and 3, the main components of the preparation apparatus include a mixing tank 100, a filter 200, and a control cabinet 300, wherein the control cabinet 300 is disposed at the front side of the filter 200.
The upper surface of the mixing tank body 100 is provided with a first liquid injection pipe 101 and a second liquid injection pipe 102 which are respectively used for adding a crude product of the aliphatic secondary alcohol polyoxyethylene ether and purified water. Be provided with the agitator 103 in the blending tank body 100, this agitator is conventional setting, includes the dwang with agitator motor 104 output shaft is connected with a large amount of stirring rods on the dwang to be provided with the agitator motor 104 that is used for driving agitator 103 in the upper end of the blending tank body 100, still be connected with a plurality of supporting legs 117 at the lower extreme circumference homogeneous connection of the blending tank body 100 simultaneously, be used for the support of whole blending tank body 100. A drain pipe 105 is connected to the lower end of the mixing tank 100, and a first manual valve 106 is provided on the drain pipe 105. When the liquids are still mixed, the first manual valve 106 can be opened to drain the water below.
Referring to fig. 4, fig. 5, fig. 6 and fig. 7, a vertical strip-shaped opening 107 is formed in the side surface of the mixing tank 100 close to the filter 200, a telescopic partition 108 is hermetically connected in the strip-shaped opening 107, and a moving block 109 is fixedly connected in the telescopic partition 108. When the telescopic interlayer 108 is specifically arranged, the telescopic interlayer 108 is made of rubber materials or plastic materials, and the moving block 109 is fixedly and hermetically connected with the telescopic interlayer 108. An oil pumping pipe 110 penetrates through the moving block 109, the inner end of the oil pumping pipe 110 is communicated with the inner cavity of the mixing tank body 100, a first electromagnetic valve 111 is arranged at the outer end of the oil pumping pipe 110, a convex block 112 is connected to the side surface of the moving block 109, and a threaded hole is formed in the convex block 112.
In addition, the outer surfaces of the mixing tank 100 above and below the lug 112 are fixedly connected with rotating seats 113, a vertically arranged screw rod 114 is connected between the two rotating seats 113, and the screw rod 114 is matched with a threaded hole on the lug 112. The outer surface of the mixing tank 100 is also provided with a screw motor 115 connected with the end of the screw 114, and the mixing tank 100 positioned beside the strip-shaped opening 107 is provided with a vertical strip-shaped glass observation window 116. In the specific setting, the length of the strip-shaped glass observation window 116 is larger than that of the strip-shaped opening 107, and the strip-shaped glass observation window 116 and the strip-shaped opening 107 are both arranged at the height position of 1001/3-2/3 of the mixing tank body. When the stirring is mixed and is kept standing for layering, an operator can penetrate through the interface of specific oil layering through the strip-shaped glass observation window 116, and then the height of the moving block 109 is adjusted through controlling the forward and reverse rotation of the screw rod motor 115 and the cooperation of the threaded hole and the screw rod 114, so that the oil pumping pipe 110 is located below an oil layer, and then the oil layer is pumped.
Referring to fig. 8, 9, 10 and 11, the filter 200 in this embodiment includes a filter box 201, wherein at least two filter assemblies 202 are disposed inside the filter box 201, and when the filter assembly 202 is disposed inside the filter box 201, 2 to 5 filter assemblies 202 may be disposed inside the filter box 201.
Referring to fig. 2, a liquid pump 203 is fixed on the side surface of the filter tank 201 close to the mixing tank 100, the liquid inlet end of the liquid pump 203 is connected with the outer end of the oil pumping pipe 110 through a hose, the liquid outlet end of the liquid pump 203 is connected with an oil delivery pipe 204, the upper end of the oil delivery pipe 204 is connected with a plurality of branch pipes 205, second electromagnetic valves 206 are arranged on the branch pipes 205, and the branch pipes 205 are connected with corresponding filter assemblies 202.
Specifically, the filter assembly 202 includes a cylinder 2021 vertically fixed in the filter box 201, a slag discharge pipe 2022 extending out of the filter box 201 is connected to the lower end of the cylinder 2021, and a second manual valve 2023 is disposed on the slag discharge pipe 2022. A hollow rotating pipe 2024 is coaxially and rotatably connected in the cylinder 2021, a driven gear 2025 is arranged at the upper end of the hollow rotating pipe 2024 extending out of the cylinder 2021, a driving motor 2026 is arranged on the upper surface of the filter box 201, a driving gear 2027 is connected to the lower end of the driving motor 2026 extending into the filter box 201, the driving gear 2027 is meshed with the driven gear 2025, and the hollow rotating pipe 2024 can be rotated by controlling the rotation of the driving motor 2026 and then by the meshing of the two gears. Meanwhile, the outer surface of the hollow rotating pipe 2024 inside the cylinder 2021 is provided with a spiral blade 2028, the upper end of the cylinder 2021 is provided with a large number of oil outlet holes 2029, the upper surface of the filter box 201 is also provided with a bearing rotatably connected with the hollow rotating pipe 2024, the top end of the hollow rotating pipe 2024 extending out of the filter box 201 is connected with a sealing rotary connecting piece 2030, and the sealing rotary connecting piece 2030 is rotatably connected with the lower end of the branch pipe 205.
Finally, an adsorbent storage bucket 204 corresponding to each filter assembly 202 is fixedly arranged on the upper surface of the filter box 201, and a large amount of activated carbon adsorbent is filled in the adsorbent storage bucket 204. The lower end of the adsorbent storage hopper 204 is connected with a material guiding channel 205, the lower end of the material guiding channel 205 is communicated with the upper end of the cylinder 2021, the lower end of the filter box 201 is provided with a material discharging pipe 206, and the material discharging pipe 206 is provided with a third manual valve 207.
The plurality of filter assemblies 202 are arranged in the filter box 201, and are usually arranged one by one, when the activated carbon adsorbent needs to be replaced after long-time filtration and impurity removal, the oil phase is controlled to be introduced into the corresponding filter assembly 202 by controlling the opening or closing of the corresponding second electromagnetic valve 206, then the oil phase enters the cylinder 2021 along the hollow rotating pipe 2024, the oil liquid flows upwards along the direction of the spiral blade 2028 under the action of continuous liquid injection, and fully contacts with the adsorbent in the flowing process to perform adsorption and impurity removal and decoloration, and finally the oil liquid is discharged from the oil outlet 2029.
When the activated carbon agent needs to be replaced and internal impurities are removed, the second manual valve 2023 is opened, the driving motor 2026 is started, all the activated carbon adsorbent is discharged through the action of the spiral blade, then the second manual valve is closed, and new activated carbon in the adsorbent storage hopper 204 is refilled through the material guide channel 205.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation device for preparing the fatty secondary alcohol polyoxyethylene ether is characterized by comprising a mixing tank body (100), a filter (200) and a control cabinet (300), wherein a first liquid injection pipe (101) and a second liquid injection pipe (102) are arranged on the upper surface of the mixing tank body (100), and a stirring frame (103) is arranged in the mixing tank body (100). A stirring motor (104) for driving a stirring rack (103) is arranged at the upper end of the mixing tank body (100), a liquid discharge pipe (105) is connected to the lower end of the mixing tank body (100), and a first manual valve (106) is arranged on the liquid discharge pipe (105);
a vertical strip-shaped opening (107) is formed in the side face, close to the filter (200), of the mixing tank body (100), a telescopic interlayer (108) is connected in the strip-shaped opening (107) in a sealing mode, a moving block (109) is fixedly connected in the telescopic interlayer (108), an oil pumping pipe (110) penetrates through the moving block (109), the inner end of the oil pumping pipe (110) is communicated with the inner cavity of the mixing tank body (100), a first electromagnetic valve (111) is arranged at the outer end of the oil pumping pipe (110), a protruding block (112) is connected to the side face of the moving block (109), a threaded hole is formed in the protruding block (112), rotating seats (113) are fixedly connected to the outer surface of the mixing tank body (100) above and below the protruding block (112), a vertically-arranged lead screw (114) is connected between the two rotating seats (113), the lead screw (114) is matched with the threaded hole in the protruding block (112), a motor (115) connected with the end portion of the lead screw (114) is further arranged on the outer surface of the mixing tank body (100), and a vertical strip-shaped glass window (116) is arranged on the mixing tank body (100) beside the strip-shaped opening (107);
the filter (200) comprises a filter box (201), at least two filter assemblies (202) are arranged in the filter box (201), a liquid pump (203) is fixed on the side face, close to the mixing tank body (100), of the filter box (201), the liquid inlet end of the liquid pump (203) is connected with the outer end of the oil pumping pipe (110) through a hose, the liquid outlet end of the liquid pump (203) is connected with an oil liquid conveying pipe (204), the upper end of the oil liquid conveying pipe (204) is connected with a plurality of branch pipes (205), second electromagnetic valves (206) are arranged on the branch pipes (205), and the branch pipes (205) are connected with the corresponding filter assemblies (202);
the filter assembly (202) comprises a cylinder (2021) vertically and fixedly arranged in a filter box (201), the lower end of the cylinder (2021) is connected with a slag discharge pipe (2022) extending out of the filter box (201), a second manual valve (2023) is arranged on the slag discharge pipe (2022), the cylinder (2021) is coaxially and rotatably connected with a hollow rotating pipe (2024), the upper end of the hollow rotating pipe (2024) extending out of the cylinder (2021) is provided with a driven gear (2025), the upper surface of the filter box (201) is provided with a driving motor (2026), the lower end of an output shaft of the driving motor (2026) extending into the filter box (201) is connected with a driving gear (2027), the driving gear (2027) is meshed with the driven gear (2025), the outer surface of the hollow rotating pipe (2024) positioned in the cylinder (2021) is provided with a spiral blade (2028), the upper end of the cylinder (2021) is provided with a large amount of oil outlet (2029), the upper surface of the filter box (201) is further provided with a rotary connecting piece (2024) rotatably connected with the hollow rotating pipe (2024), and the lower end of the hollow rotating pipe (2021) is rotatably connected with a sealing connecting piece (2030);
the upper surface of rose box (201) still fixed be provided with adsorbent storage bucket (204) that each filtering component (202) corresponds, the lower extreme of adsorbent storage bucket (204) is connected with guide passageway (205), the lower extreme of guide passageway (205) is linked together with the upper end of drum (2021), the lower extreme of rose box (201) is provided with row material pipe (206), and is provided with third manual valve (207) on arranging material pipe (206).
2. The preparation device in the preparation method of the aliphatic secondary alcohol polyoxyethylene ether according to claim 1, wherein a plurality of supporting legs (117) are uniformly connected to the lower end of the mixing tank body (100) in the circumferential direction.
3. The preparation device in the preparation method of the aliphatic secondary alcohol polyoxyethylene ether according to claim 1, wherein the stirring frame (103) comprises a rotating rod connected with an output shaft of the stirring motor (104), and a large number of stirring rods are connected on the rotating rod.
4. The preparation device in the preparation method of the aliphatic secondary alcohol polyoxyethylene ether according to claim 1, wherein the telescopic interlayer (108) is made of a rubber material or a plastic material, and the moving block (109) is fixedly and hermetically connected with the telescopic interlayer (108).
5. The preparation device in the preparation method of the aliphatic secondary alcohol polyoxyethylene ether according to claim 1, wherein the number of the filter assemblies (202) arranged inside the filter box (201) is 2-5.
6. The preparation device in the preparation method of the aliphatic secondary alcohol polyoxyethylene ether according to claim 1, wherein the strip-shaped glass observation window (116) is arranged to be longer than the strip-shaped opening (107), and the strip-shaped glass observation window (116) and the strip-shaped opening (107) are both arranged at a height position of 1/3-2/3 of the mixing tank body (100).
7. The apparatus for preparing fatty secondary alcohol polyoxyethylene ether according to claim 1, wherein the adsorbent storage hopper (204) is filled with a large amount of activated carbon adsorbent.
8. A method for producing an aliphatic secondary alcohol polyoxyethylene ether by using the production apparatus according to any one of claims 1 to 7,
s1: carrying out contact reaction on secondary alcohol and ethylene oxide under the action of an acid catalyst to obtain a crude product of fatty secondary alcohol polyoxyethylene ether;
s2, transferring the crude product of the aliphatic secondary alcohol polyoxyethylene ether into a mixing tank body (100) in the preparation device, adding water, stirring, and then standing for layering;
s3: after the mixed liquid is kept stand and layered, pumping the oil phase into a filter (200) in the preparation device for adsorption, impurity removal and decoloration;
s4: and pumping the liquid after impurity removal and decoloration into a rectifying still for rectification to obtain the fatty secondary alcohol polyoxyethylene ether.
9. The method for preparing fatty secondary alcohol polyoxyethylene ether according to claim 8, wherein the acidic catalyst in step 1 is H 2 SO 4 、HClO 4 And anhydrous stannic chloride or aluminum chloride.
10. The method for preparing aliphatic secondary alcohol polyoxyethylene ether according to claim 9, wherein the rectification temperature in the step 4 is controlled within the range of 40-48 ℃.
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Denomination of invention: Preparation method and device of fatty secondary alcohol polyoxyethylene ether Granted publication date: 20230428 Pledgee: Bank of Nanjing Co.,Ltd. Lianyungang Branch Pledgor: JISANGSU SECOL CHEMICAL Co. Registration number: Y2024980005061 |
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