CN114437327A - Preparation method and preparation device of hydrophilic polyester polyol containing lateral methyl - Google Patents
Preparation method and preparation device of hydrophilic polyester polyol containing lateral methyl Download PDFInfo
- Publication number
- CN114437327A CN114437327A CN202210136585.4A CN202210136585A CN114437327A CN 114437327 A CN114437327 A CN 114437327A CN 202210136585 A CN202210136585 A CN 202210136585A CN 114437327 A CN114437327 A CN 114437327A
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- China
- Prior art keywords
- cavity
- polyester polyol
- hydrophilic polyester
- bearing
- bottle
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- 229920005906 polyester polyol Polymers 0.000 title claims abstract description 27
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 17
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 45
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 14
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 230000007246 mechanism Effects 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 4
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 6
- 230000009969 flowable effect Effects 0.000 abstract 1
- 229920002635 polyurethane Polymers 0.000 description 14
- 239000004814 polyurethane Substances 0.000 description 14
- 238000001723 curing Methods 0.000 description 6
- 238000005381 potential energy Methods 0.000 description 5
- 238000013008 moisture curing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920003009 polyurethane dispersion Polymers 0.000 description 1
Images
Classifications
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- 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
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The application discloses a preparation method of hydrophilic polyester polyol containing lateral methyl and a preparation device thereof, comprising the following steps: sequentially adding alcohol, carboxylic acid and antioxidant into a four-neck flask according to the proportion, heating and charging nitrogen for protection; gradually heating the four-neck flask, stirring after the raw materials are completely melted, heating the four-neck flask to 130-170 ℃, keeping the temperature for 1 hour, and then entering the step; continuing to heat to 215 ℃ until the water is removed to more than 95%, sampling and analyzing the acid value, and entering the step after the acid value is less than 20 mgKOH/g; adding a catalyst, keeping the reaction temperature, gradually reducing the vacuum to-0.1 MPa, sampling and analyzing the acid value and the hydroxyl value to reach technical parameters, and then entering the step; when the temperature of the material is reduced to 90-100 ℃, packaging for later use, the technical parameters of the obtained new hydrophilic polyester polyol material containing lateral methyl are as follows: 1) at room temperature (25 ℃), a low-viscosity, flowable, clear liquid; 2) acid value is less than 1.0, OH (hydroxyl value) is between 33 and 118mgKOH/g (molecular weight is between 1000 and 3000), moisture content is less than 500PPm, and color number is less than 50.
Description
Technical Field
The invention relates to a preparation method and a preparation device of hydrophilic polyester polyol containing lateral methyl.
Background
In recent years, with the rapid development of solvent-free polyurethane and environment-friendly polyurethane, the solvent-free polyurethane and the environment-friendly polyurethane have increasingly large market potential and are more and more abundant in variety. Therefore, the market demand for liquid low-viscosity polyester polyol having good fluidity at normal temperature is enormous. The polyester polyol has low viscosity and good fluidity at normal temperature, and the hydrophilic group of the polyester polyol can well promote the curing and curing of polyurethane by using solvent-free moisture curing polyurethane synthesized by the polyester polyol, and the polyurethane has no solvent and the like so as to obtain excellent adhesion, so the polyester polyol is named as side methyl hydrophilic polyester polyol. Can be widely applied to the fields of solvent-free polyurethane, moisture curing polyurethane, aqueous polyurethane dispersion, solvent type polyurethane adhesive and the like, so that improvement is needed.
Disclosure of Invention
The present invention is directed to solving one of the technical problems of the prior art.
The application provides a preparation method of hydrophilic polyester polyol containing lateral methyl, which is characterized by comprising the following steps:
s1, sequentially putting alcohol, carboxylic acid and an antioxidant into a four-neck flask according to the proportion, heating and filling nitrogen for protection;
s2, gradually heating the four-neck flask, stirring after the raw materials are completely melted, heating the four-neck flask to 130-170 ℃, keeping the temperature for 1 hour, and entering the step S3;
s3, continuing to heat to 215 ℃ until the water is removed to more than 95%, sampling and analyzing the acid value, and entering the step S4 when the acid value is less than 20 mgKOH/g;
s4, adding a catalyst, keeping the reaction temperature, gradually reducing the vacuum to-0.1 MPa, sampling and analyzing the acid value and the hydroxyl value to reach technical parameters, and then entering the step S5;
s5, cooling the materials to 90-100 ℃, and packaging for later use;
wherein the grams of alcohol, carboxylic acid and antioxidant are 469.5, 584 and 0.25 respectively.
Further comprising:
the carboxylic acid is mainly aliphatic carboxylic acid and accounts for about 70 to 100 percent of the total mass of the carboxylic acid; aromatic carboxylic acid is taken as an auxiliary material, and accounts for about 0-20% of the total weight; aliphatic is preferably adipic acid, succinic acid, etc.; aromatic compounds such as phthalic anhydride and isophthalic acid; one or more than two of the above-mentioned materials.
Further comprising:
the alcohol comprises ethylene glycol, diethylene glycol and polyethylene glycol;
wherein the mass of the ethylene glycol, the diethylene glycol and the polyethylene glycol is 156.5g respectively.
The method comprises the following steps:
the four-mouth flask comprises a flask body, a stirring device, a vacuumizing tube and a plurality of bottle mouths;
the bearing table comprises a pedestal, a bearing cavity, a heating wire and a cooling unit;
wherein, bearing the weight of the chamber and being arranged in holding the weight of the platform and being used for holding the body, the heating wire is installed in bearing the weight of the intracavity, agitating unit stretches into in the body through one of them bottleneck, evacuation pipe and one of them bottleneck intercommunication, cooling unit are used for supplying the air current to the bearing the weight of the intracavity and cooling down the body.
Also disclosed is a device for preparing hydrophilic polyester polyol containing pendant methyl groups, the pedestal comprising:
a seat body in an L shape;
the bottom end of the side plate is hinged between one side of the bottom of the seat body and the seat body to form a bearing cavity;
the pair of arc-shaped stop blocks are respectively arranged at the tops of the side plates and the seat body, and the bottom surfaces of the arc-shaped stop blocks are abutted against the outer wall of the bottle body when the side plates are folded;
and the locking mechanism is used for detachably connecting the pair of arc-shaped stop blocks.
The locking mechanism includes:
the slot is arranged at the top of the right arc-shaped stop block;
one end of the connecting plate is fixedly connected with the right arc-shaped stop block, and the other end of the connecting plate is inserted into the slot when the side plates are folded;
the telescopic piece is movably arranged on the connecting plate;
and the clamping block is fixedly arranged at the top of the movable end of the connecting plate and is in clamping fit with the telescopic piece to fix the movable end of the connecting plate.
The expansion piece includes:
the clamping groove penetrates through the movable end of the connecting plate from top to bottom;
the bottom end of the anti-falling rod is fixedly arranged at the bottom end of the slot, and the top end of the anti-falling rod movably penetrates through the slot and extends upwards;
the sleeve is sleeved at the top end of the anti-falling rod;
the sliding block is arranged at the top end of the anti-falling rod and is arranged in the inner cavity of the sleeve in a sliding manner;
and the first spring is sleeved on the outer side of the anti-falling rod and is positioned between the bottom surface of the sliding block and the bottom end of the inner cavity of the sleeve.
The cooling unit includes:
the cooling cavity is arranged in the pedestal and wraps the bearing cavity;
the air inlet pipe is provided with a first valve and is communicated with the cooling cavity;
and the air outlet holes are used for communicating the cooling cavity with the bearing cavity.
Further comprising:
the first three-way valve is arranged on the vacuumizing pipe;
the second valve is arranged on the vacuumizing pipe and is far away from the bottle opening and the first three-way valve;
the second three-way valve is arranged on the air inlet pipe and is positioned between the pedestal and the first valve;
two ends of the communicating pipe are communicated with the first three-way valve and the second three-way valve;
and the plurality of one-way air outlet units are used for preventing air in the bearing cavity from entering the cooling cavity through the air outlet holes.
The one-way air outlet unit comprises:
the mounting screw hole is arranged on the inner wall of the bearing cavity and communicated with the air outlet hole;
the outer wall of the supporting block is provided with threads and is connected with the mounting screw holes through the threads;
the non-return cavity is arranged at the bottom of the mounting screw hole and communicated with the air outlet;
one end of the exhaust pipe is communicated with one end of the check cavity, which is far away from the check cavity, and the other end of the exhaust pipe is communicated with the top of the side wall of the supporting block;
the steel ball is arranged in the non-return cavity, and the diameter of the steel ball is smaller than the cross section area of the non-return cavity;
and the spring II is used for abutting the outer wall of the steel ball with the air outlet.
The invention has the following main beneficial effects:
1. the technical parameters of the new hydrophilic polyester polyol material containing the lateral methyl prepared by the method are as follows:
1) the low-viscosity liquid can flow into a transparent liquid state at room temperature;
2) acid value is less, OH hydroxyl value is between-mgKOH/g, namely molecular weight is-between, moisture content is less than PPm, and color number is less;
the advantages are as follows:
1) containing pendant methyl, hydrophilic groups;
2) the curing and curing performance requirements of solvent-free polyurethane, moisture curing polyurethane and the like are met, and the production efficiency is improved.
2. The closed side plates are fixed through the matching of the sleeve, the first spring, the piston, the anti-falling rod, the arc-shaped stop blocks, the inserting grooves and the clamping grooves, and the bottom surfaces of the arc-shaped stop plates on the two sides are abutted to the outer wall of the bottle body, so that the bottle body can be conveniently mounted and taken out, the stability of the bottle body is improved, and the phenomenon that the bottle body is toppled to cause danger is avoided;
3. cooling airflow is introduced into the bearing cavity through the arrangement of the cooling cavity, the air inlet pipe, the first valve and the air outlet holes, and flows through the surface of the bottle body to quickly cool the bottle body;
4. through the arrangement of the first three-way valve, the second three-way valve, the mounting screw hole, the supporting block, the non-return cavity, the exhaust pipe, the steel ball, the second spring and the communicating pipe, when the bottle body needs to be kept warm, the first valve is closed, the second valve is opened, the first three-way valve is adjusted to enable the air inlet pipe and the communicating pipe to be communicated with the vacuum pumping pipe, air in the cooling cavity can be discharged, the interior of the cooling cavity is enabled to be true, the heat preservation effect is improved, when materials in the bottle body need to be cooled, the first valve is opened, the second three-way valve is adjusted to enable the air inlet pipe to be communicated, cooling air flow enters the cooling cavity through the air inlet pipe, air pressure in the cooling cavity is increased to jack up the non-return cavity for the steel ball, elastic potential energy is stored in the second spring, the air flow in the cooling cavity enters between the inner wall of the bearing cavity and the bottle body after passing through the air outlet hole, the non-return cavity and the exhaust pipe, is discharged from the top of the bearing cavity after flowing through the surface of the bottle body, the air flow is cooled, through such a mode, improve the heat preservation effect and the cooling rate to the body.
Drawings
FIG. 1 is a schematic diagram of a specific structure of an apparatus for preparing a hydrophilic polyester polyol containing pendant methyl groups according to an embodiment of the present application;
FIG. 2 is an enlarged view of a portion A of FIG. 1;
fig. 3 is a schematic view of a part B of fig. 1.
Reference numerals
1-bottle body, 2-stirring device, 3-vacuumizing tube, 4-bottle mouth, 5-pedestal, 501-seat body, 502-side plate, 503-arc baffle, 6-bearing cavity, 7-heating wire, 8-cooling unit, 801-cooling cavity, 802-air inlet tube, 803-air outlet hole, 804-three-way valve I, 805-valve I, 806-valve II, 807-three-way valve II, 808-communicating tube, 9-locking mechanism, 901-slot, 902-connecting plate, 903-telescopic part, 9031-clamping groove, 9032-anti-falling rod, 9033-sleeve, 9034-sliding block, 9035-spring I, 904-clamping block, 10-one-way air outlet unit, 1001-mounting screw hole, 1002-supporting block, 1003-a non-return cavity, 1004-an exhaust pipe, 1005-a steel ball and 1006-a second spring.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, embodiments of the present application. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present disclosure.
The terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It will be appreciated that the data so used may be interchanged under appropriate circumstances such that embodiments of the application may be practiced in sequences other than those illustrated or described herein, and that the terms "first," "second," and the like are generally used herein in a generic sense and do not limit the number of terms, e.g., the first term can be one or more than one. In addition, "and/or" in the specification and claims means at least one of connected objects, a character "/" generally means that a preceding and succeeding related objects are in an "or" relationship.
The server provided by the embodiment of the present application is described in detail below with reference to the accompanying drawings through specific embodiments and application scenarios thereof.
The application provides a preparation method of hydrophilic polyester polyol containing lateral methyl, which is characterized by comprising the following steps:
s1, sequentially putting alcohol, carboxylic acid and an antioxidant into a four-neck flask according to the proportion, heating and filling nitrogen for protection;
s2, gradually heating the four-neck flask, stirring after the raw materials are completely melted, heating the four-neck flask to 130-170 ℃, keeping the temperature for 1 hour, and entering the step S3;
s3, continuing to heat to 215 ℃ until the water is removed to more than 95%, sampling and analyzing the acid value, and entering the step S4 when the acid value is less than 20 mgKOH/g;
s4, adding a catalyst, keeping the reaction temperature, gradually reducing the vacuum to-0.1 MPa, sampling and analyzing the acid value and the hydroxyl value to reach technical parameters, and then entering the step S5;
s5, cooling the materials to 90-100 ℃, and packaging for later use;
wherein the grams of alcohol, carboxylic acid and antioxidant are 469.5, 584 and 0.25 respectively.
In the embodiment of the application, the preparation method and the preparation device of the hydrophilic polyester polyol containing the lateral methyl are adopted,
further: the carboxylic acid is mainly aliphatic carboxylic acid and accounts for about 70 to 100 percent of the total mass of the carboxylic acid; aromatic carboxylic acid is taken as an auxiliary material, and accounts for about 0-20% of the total weight; aliphatic is preferably adipic acid, succinic acid, etc.; aromatic compounds such as phthalic anhydride and isophthalic acid; one or more than two of the above-mentioned materials.
In the present embodiment, the above-described structure is adopted.
Further: the alcohol comprises ethylene glycol, diethylene glycol and polyethylene glycol;
wherein the mass of the ethylene glycol, the diethylene glycol and the polyethylene glycol is 156.5g respectively.
In the embodiment, due to the adoption of the method, the technical parameters of the obtained new hydrophilic polyester polyol material containing the lateral methyl are as follows:
1) the low-viscosity liquid can flow into a transparent liquid state at the room temperature of 25 ℃;
2) the acid value is less than 1.0, the OH hydroxyl value is between 33 and 118mgKOH/g, namely the molecular weight is between 1000-3000, the moisture content is less than 500PPm, and the color number is less than 50;
the advantages are as follows:
1) containing pendant methyl, hydrophilic groups;
2) the curing and curing performance requirements of solvent-free polyurethane, moisture curing polyurethane and the like are met, and the production efficiency is improved.
As shown in fig. 1 to 3, there is also disclosed a device for preparing a hydrophilic polyester polyol containing pendant methyl groups, comprising: the four-neck flask comprises a flask body 1, a stirring device 2, a vacuumizing pipe 3 and a plurality of flask mouths 4; the plummer, it includes pedestal 5, bears chamber 6, heating wire 7 and cooling unit 8, bears chamber 6 and is arranged in holding the plummer and is used for holding body 1, and heating wire 7 is installed in bearing chamber 6, and agitating unit 2 stretches into body 1 through one of them bottleneck 4 in, and evacuation pipe 3 communicates with one of them bottleneck 4, and cooling unit 8 is used for cooling down body 1 to the air current that supplies in bearing chamber 6.
Further, the pedestal 5 includes: a base 501, which is L-shaped; the bottom end of the side plate 502 is hinged to one side of the bottom of the seat body 501, and a bearing cavity 6 is formed between the seat body 501 and the side of the bottom of the seat body 501; a pair of arc-shaped stoppers 503 which are respectively arranged on the top of the side plate 502 and the base 501 and the bottom surface of which is abutted against the outer wall of the bottle body 1 when the side plate 502 is folded; and a locking mechanism 9 for detachably connecting the pair of arc-shaped stoppers 503.
Further, the locking mechanism 9 includes: a slot 901 disposed at the top of the right arc-shaped stopper 503; one end of the connecting plate 902 is fixedly connected with the right arc-shaped stop 503, and the other end is inserted into the slot 901 when the side plate 502 is folded; a telescopic member 903 movably mounted on the connecting plate 902; and a clamping block 904 which is fixedly arranged at the top of the movable end of the connecting plate 902 and is in clamping fit with the telescopic piece 903 to fix the movable end of the connecting plate 902.
Further, the telescopic member 903 includes: a clamping groove 9031 penetrates through the movable end of the connecting plate 902 from top to bottom; the bottom end of the anti-falling rod 9032 is fixedly installed at the bottom end of the slot 901, and the top end of the anti-falling rod is movably inserted through the slot 9031 to extend upwards; a sleeve 9033, which is sleeved on the top end of the anti-drop rod 9032; a sliding block 9034 which is installed at the top end of the anti-falling rod 9032 and is installed in the inner cavity of the sleeve 9033 in a sliding mode; the first spring 9035 is sleeved on the outer side of the anti-falling rod 9032 and is located between the bottom surface of the sliding block 9034 and the bottom end of the inner cavity of the sleeve 9033.
Further, the cooling unit 8 includes: a cooling chamber 801 disposed in the pedestal 5 and enclosing the bearing chamber 6; an air inlet pipe 802 which is provided with a first valve 805 and is communicated with the cooling cavity 801; and a plurality of air outlet holes 803 are used for communicating the cooling cavity 801 with the bearing cavity 6.
Further, the method also comprises the following steps: the three-way valve I804 is arranged on the vacuum pumping pipe 3; a second valve 806 mounted on the evacuation tube 3 remote from the mouth 4 and the first three-way valve 804; a second three-way valve 807 mounted on the inlet pipe 802 between the pedestal 5 and the first valve 805; a communication pipe 808, both ends of which communicate the first three-way valve 804 and the second three-way valve 807; and a plurality of one-way air outlet units 10 for preventing the air in the bearing cavity 6 from entering the cooling cavity 801 through the air outlet holes 803.
Further, the unidirectional air outlet cell 10 includes: a mounting screw hole 1001 which is arranged on the inner wall of the bearing cavity 6 and communicated with the air outlet 803; a support block 1002, the outer wall of which is threaded and is connected with the mounting screw hole 1001 through threads; a non-return cavity 1003 arranged at the bottom of the mounting screw hole 1001 and communicated with the air outlet 803; an exhaust pipe 1004, one end of which is communicated with one end of the non-return cavity 1003 far away from the non-return cavity 1003, and the other end of which is communicated with the top of the side wall of the supporting block 1002; a steel ball 1005 which is arranged in the non-return cavity 1003 and has a diameter smaller than the cross-sectional area of the non-return cavity 1003; and a second spring 1006 for abutting the outer wall of the steel ball 1005 with the air outlet 803.
In the preferred embodiment, due to the above structure, the sleeve 9033 is pulled in the direction away from the base 501, the first spring 9035 is compressed to store elastic potential energy, the outer wall of the sleeve 9033 is separated from the contact with the fixture block 904, the side plate 502 is turned over, the movable end of the connecting plate 902 is separated from the slot 901, one side of the bearing cavity 6 is opened, the bottle body 1 is placed into the bearing cavity 6 and erected on each supporting block 1002, the side plate 502 is turned over to close one side of the bearing cavity 6, the movable end of the connecting plate 902 is inserted into the slot 901, the anti-falling rod 9032 enters the slot 9031, the sleeve 9033 is loosened, the first spring 9035 loses external force and releases elastic potential energy to generate kinetic energy, the sleeve 9033 descends by matching with gravity, the outer wall abuts against the fixture block 904, the movable end of the connecting plate 902 is fixed, the side plate 502 is fixed, a material is put into the bottle body 1 through the bottle mouth 4, the bottle mouth 4 is closed, the electric heating wire 7 is electrified to generate heat, and the first valve 805 is closed, Opening a second valve 806, adjusting a first three-way valve 804 to enable an air inlet pipe 802 and a communicating pipe 808 to be communicated with a vacuumizing pipe 3, discharging air in the cooling cavity 801, adjusting the first three-way valve 804 to enable the air inlet pipe 802 and the communicating pipe 808 to be disconnected after the air in the cooling cavity 801 is vacuumized, closing a first valve 805, opening a second valve 806 after the acid value of materials in the bottle body is less than 20mgKOH/g, discharging the gas in the bottle body 1 through a bottle opening 4 and the vacuumizing pipe 3 until the vacuum in the bottle body 1 reaches-0.1 MPa, closing the second valve 806, powering off a heating wire 7 after the acid value and the hydroxyl value reach technical parameters, opening the first valve 805, adjusting a second three-way valve 807 to enable the air inlet pipe 802 to be connected, enabling cooling air flow to enter the cooling cavity 801 through the air inlet pipe 802, lifting up a steel ball 1005 in a non-return cavity 1003 when the pressure in the cooling cavity 801 rises, storing elastic potential energy through a second spring 1006, enabling the air flow in the cooling cavity 801 to be shortened, and enabling the air flow 803 to pass through a hole 803, Check and get into behind chamber 1003 and the blast pipe 1004 and bear between 6 inner walls of chamber and the body 1, flow through body 1 surface and discharge from bearing 6 tops of chamber, cool down body 1 through the air current, when treating that the material temperature in the body 1 reduces to 90 ~ 100 ℃, with sleeve 9033 to the direction pulling of keeping away from pedestal 501, spring 9035 pressurized shortens deposit elastic potential energy, sleeve 9033 outer wall breaks away from the contact with fixture block 904, overturn curb plate 502, the expansion end of connecting plate 902 breaks away from slot 901, bear 6 one side of chamber and open, the staff dresses thermal-insulated gloves and takes out body 1 from bearing chamber 6, take out the packing spare through bottleneck 4 with the material.
Preferably, the maximum diameter of the bottle body 1 is smaller than the cross-sectional area of the open side of the bearing cavity 6 when the side plate 502 is opened, so that the bottle body 1 can normally enter and exit the bearing cavity 6, and since the side plate 502 is arranged on one side of the seat body 501, as shown in fig. 1, when the side plate 502 is turned over to open the bearing cavity 6, the bottle body 1 cannot fall out of the bearing cavity 6 and be damaged.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. Further, it should be noted that the scope of the methods and apparatus of the embodiments of the present application is not limited to performing the functions in the order illustrated or discussed, but may include performing the functions in a substantially simultaneous manner or in a reverse order based on the functions involved, e.g., the methods described may be performed in an order different than that described, and various steps may be added, omitted, or combined. Additionally, features described with reference to certain examples may be combined in other examples.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of hydrophilic polyester polyol containing lateral methyl is characterized by comprising the following steps:
s1, sequentially putting alcohol, carboxylic acid and an antioxidant into a four-neck flask according to the proportion, heating and filling nitrogen for protection;
s2, gradually heating the four-neck flask, stirring after the raw materials are completely melted, heating the four-neck flask to 130-170 ℃, keeping the temperature for 1 hour, and entering the step S3;
s3, continuing to heat to 215 ℃ until the water is removed to more than 95%, sampling and analyzing the acid value, and entering the step S4 when the acid value is less than 20 mgKOH/g;
s4, adding a catalyst, keeping the reaction temperature, gradually reducing the vacuum to-0.1 MPa, sampling and analyzing the acid value and the hydroxyl value to reach technical parameters, and then entering the step S5;
s5, cooling the materials to 90-100 ℃, and packaging for later use;
wherein the grams of the alcohol, the carboxylic acid and the antioxidant are 469.5, 584 and 0.25 respectively.
2. The method of claim 1, further comprising:
the carboxylic acid is mainly aliphatic carboxylic acid and accounts for 70-100% of the total mass of the carboxylic acid; aromatic carboxylic acid is used as an auxiliary material, and accounts for about 0-20% of the total weight; aliphatic is preferably adipic acid, succinic acid, etc.; aromatic compounds such as phthalic anhydride and isophthalic acid; one or more than two of the above-mentioned materials.
3. The method of claim 1, further comprising:
the alcohol comprises ethylene glycol, diethylene glycol and polyethylene glycol which are mixed with each other;
wherein the mass of the ethylene glycol, the diethylene glycol and the polyethylene glycol is 156.5g respectively.
4. A device for preparing the hydrophilic polyester polyol containing pendant methyl groups according to any one of claims 1 to 3, comprising:
the four-mouth flask comprises a flask body (1), a stirring device (2), a vacuumizing tube (3) and a plurality of bottle mouths (4);
the bearing table comprises a pedestal (5), a bearing cavity (6), a heating wire (7) and a cooling unit (8);
the vacuum bottle comprises a bearing cavity (6), an electric heating wire (7), a stirring device (2), a vacuum pumping pipe (3), a bottle body (1), a cooling unit (8) and a bottle body (1), wherein the bearing cavity (6) is located in the bearing platform and used for accommodating the bottle body (1), the electric heating wire (7) is installed in the bearing cavity (6), the stirring device (2) stretches into the bottle body (1) through one of the bottle openings (4), the vacuum pumping pipe is communicated with one of the bottle openings (4), and the cooling unit (8) is used for supplying air flow into the bearing cavity (6) to cool the bottle body (1).
5. The apparatus for preparing hydrophilic polyester polyol containing pendant methyl groups according to claim 4, wherein said stand (5) comprises:
a base body (501) which is L-shaped;
the bottom end of the side plate (502) is hinged to one side of the bottom of the seat body (501) and forms a bearing cavity (6) with the seat body (501);
the pair of arc-shaped stop blocks (503) are respectively arranged at the tops of the side plate (502) and the base body (501), and the bottom surfaces of the arc-shaped stop blocks are abutted against the outer wall of the bottle body (1) when the side plate (502) is folded;
and the locking mechanism (9) is used for detachably connecting the pair of arc-shaped stop blocks (503).
6. The device for preparing hydrophilic polyester polyols containing pendant methyl groups according to claim 5, wherein the locking mechanism (9) comprises:
the inserting groove (901) is arranged at the top of the arc-shaped stop block (503) at the right side;
one end of the connecting plate (902) is fixedly connected with the arc-shaped stop block (503) at the right side, and the other end of the connecting plate is inserted into the slot (901) when the side plates (502) are folded;
a telescopic member (903) movably mounted on the connecting plate (902);
and the clamping block (904) is fixedly arranged at the top of the movable end of the connecting plate (902) and is in clamping fit with the telescopic piece (903) to fix the movable end of the connecting plate (902).
7. The apparatus for preparing hydrophilic polyester polyol containing pendant methyl groups according to claim 6, wherein the extension member (903) comprises:
the clamping groove (9031) penetrates through the movable end of the connecting plate (902) from top to bottom;
the bottom end of the anti-falling rod (9032) is fixedly installed at the bottom end of the slot (901), and the top end of the anti-falling rod movably penetrates through the slot (9031) to extend upwards;
the sleeve (9033) is sleeved at the top end of the anti-falling rod (9032);
the sliding block (9034) is installed at the top end of the anti-falling rod (9032) and is installed in the inner cavity of the sleeve (9033) in a sliding mode;
the first spring (9035) is sleeved on the outer side of the anti-falling rod (9032) and is located between the bottom surface of the sliding block (9034) and the bottom end of the inner cavity of the sleeve (9033).
8. The apparatus for preparing hydrophilic polyester polyol containing pendant methyl groups according to claim 4, wherein the cooling unit (8) comprises:
a cooling cavity (801) which is arranged in the pedestal (5) and wraps the bearing cavity (6);
an air inlet pipe (802) provided with a first valve (805) and communicated with the cooling cavity (801);
a plurality of air outlet holes (803) for communicating the cooling cavity (801) and the bearing cavity (6).
9. The apparatus for preparing hydrophilic polyester polyol containing pendant methyl groups according to claim 8, wherein the cooling unit (8) further comprises:
a first three-way valve (804) mounted on the evacuation tube (3);
the second valve (806) is arranged on the vacuumizing pipe (3) and is far away from the bottle opening (4) and the first three-way valve (804);
a second three-way valve (807) mounted on the inlet pipe (802) between the pedestal (5) and the first valve (805);
a communication pipe (808), two ends of which are communicated with the first three-way valve (804) and the second three-way valve (807);
and the unidirectional air outlet units (10) are used for preventing the air in the bearing cavity (6) from entering the cooling cavity (801) through the air outlet holes (803).
10. The apparatus for preparing hydrophilic polyester polyol containing pendant methyl groups according to claim 9, wherein the unidirectional gas outlet unit (10) comprises:
the mounting screw hole (1001) is arranged on the inner wall of the bearing cavity (6) and communicated with the air outlet hole (803);
the supporting block (1002), its outer wall has whorls and passes the threaded connection with mounting screw (1001);
the non-return cavity (1003) is arranged at the bottom of the mounting screw hole (1001) and communicated with the air outlet hole (803);
one end of the exhaust pipe (1004) is communicated with one end, far away from the non-return cavity (1003), of the non-return cavity (1003), and the other end of the exhaust pipe is communicated with the top of the side wall of the supporting block (1002);
the steel ball (1005) is arranged in the non-return cavity (1003) and has a diameter smaller than the cross section area of the non-return cavity (1003);
and a second spring (1006) for abutting the outer wall of the steel ball (1005) with the air outlet hole (803).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210136585.4A CN114437327A (en) | 2022-02-15 | 2022-02-15 | Preparation method and preparation device of hydrophilic polyester polyol containing lateral methyl |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210136585.4A CN114437327A (en) | 2022-02-15 | 2022-02-15 | Preparation method and preparation device of hydrophilic polyester polyol containing lateral methyl |
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Citations (4)
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|---|---|---|---|---|
| CN102492126A (en) * | 2011-12-06 | 2012-06-13 | 廊坊开发区斯科瑞聚氨酯有限公司 | Method and device for producing polyester polyol |
| CN104650330A (en) * | 2013-11-18 | 2015-05-27 | 上海凯众材料科技股份有限公司 | Preparation method of polyester dihydric alcohol and microcellular polyurethane elastomer |
| CN106633018A (en) * | 2016-12-30 | 2017-05-10 | 上海聚友化工有限公司 | Continuous production process and continuous production device for polyester polyol |
| CN107400205A (en) * | 2017-07-19 | 2017-11-28 | 东莞市左镕工实业有限公司 | A kind of elastic resin and preparation method thereof |
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2022
- 2022-02-15 CN CN202210136585.4A patent/CN114437327A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492126A (en) * | 2011-12-06 | 2012-06-13 | 廊坊开发区斯科瑞聚氨酯有限公司 | Method and device for producing polyester polyol |
| CN104650330A (en) * | 2013-11-18 | 2015-05-27 | 上海凯众材料科技股份有限公司 | Preparation method of polyester dihydric alcohol and microcellular polyurethane elastomer |
| CN106633018A (en) * | 2016-12-30 | 2017-05-10 | 上海聚友化工有限公司 | Continuous production process and continuous production device for polyester polyol |
| CN107400205A (en) * | 2017-07-19 | 2017-11-28 | 东莞市左镕工实业有限公司 | A kind of elastic resin and preparation method thereof |
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