CN114456361B - Modified water-resistant resin and preparation method thereof - Google Patents
Modified water-resistant resin and preparation method thereof Download PDFInfo
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- CN114456361B CN114456361B CN202210203341.3A CN202210203341A CN114456361B CN 114456361 B CN114456361 B CN 114456361B CN 202210203341 A CN202210203341 A CN 202210203341A CN 114456361 B CN114456361 B CN 114456361B
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- 229920005989 resin Polymers 0.000 title claims abstract description 59
- 239000011347 resin Substances 0.000 title claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 116
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 105
- 238000005070 sampling Methods 0.000 claims abstract description 103
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 51
- 230000001105 regulatory effect Effects 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 45
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 16
- 239000003085 diluting agent Substances 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 13
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims abstract description 13
- LNYYKKTXWBNIOO-UHFFFAOYSA-N 3-oxabicyclo[3.3.1]nona-1(9),5,7-triene-2,4-dione Chemical compound C1=CC(C(=O)OC2=O)=CC2=C1 LNYYKKTXWBNIOO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000010926 purge Methods 0.000 claims abstract description 6
- 238000010790 dilution Methods 0.000 claims description 36
- 239000012895 dilution Substances 0.000 claims description 36
- 238000011049 filling Methods 0.000 claims description 19
- 238000007865 diluting Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 5
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- BVFSYZFXJYAPQJ-UHFFFAOYSA-N butyl(oxo)tin Chemical compound CCCC[Sn]=O BVFSYZFXJYAPQJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 27
- 229920006337 unsaturated polyester resin Polymers 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000002928 artificial marble Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- 239000002969 artificial stone Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- XESZUVZBAMCAEJ-UHFFFAOYSA-N 4-tert-butylcatechol Chemical compound CC(C)(C)C1=CC=C(O)C(O)=C1 XESZUVZBAMCAEJ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229940120693 copper naphthenate Drugs 0.000 description 1
- SEVNKWFHTNVOLD-UHFFFAOYSA-L copper;3-(4-ethylcyclohexyl)propanoate;3-(3-ethylcyclopentyl)propanoate Chemical compound [Cu+2].CCC1CCC(CCC([O-])=O)C1.CCC1CCC(CCC([O-])=O)CC1 SEVNKWFHTNVOLD-UHFFFAOYSA-L 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 1
- 238000010125 resin casting Methods 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
-
- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
- C08G63/54—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation the acids or hydroxy compounds containing carbocyclic rings
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a modified water-resistant resin and a preparation method thereof, wherein the raw materials of the modified water-resistant resin comprise maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol, a catalyst, a polymerization inhibitor and a diluent, the preparation method of the modified water-resistant resin adopts a reaction system for resin production to continuously produce and prepare the modified water-resistant resin, and the prepared modified water-resistant resin has the advantages of good strong acid corrosion resistance, good strong alkali corrosion resistance and good hydrolytic stability; in the process of forming the nitrogen atmosphere in the reaction kettle, the preparation method can utilize nitrogen to purge the feeding device, so that residual raw materials in the feeding device are avoided, and when the reaction kettle is in a vacuum state, the preparation method can send the raw materials into the reaction kettle without destroying the vacuum state of the reaction kettle, so that isobaric feeding is realized, and differential pressure sampling of materials in the reaction kettle can be realized through the vacuum pump, the pressure regulating pipeline and the sampling device.
Description
Technical Field
The invention relates to the technical field of unsaturated polyester resin, in particular to modified water-resistant resin and a preparation method thereof.
Background
The unsaturated polyester resin is thermosetting resin formed by condensation polymerization of saturated dihydric alcohol, saturated acid and unsaturated dibasic acid (or anhydride), and has the advantages of good mechanical property, electrical property and chemical corrosion resistance, easily available raw materials, simple processing technology and the like, so the unsaturated polyester resin is widely applied to various fields of artificial stone processing, glass fiber reinforced materials, chemical corrosion prevention, casting products, sanitary furniture, artware manufacturing and the like, and becomes an important thermosetting resin material.
Chinese patent application No. 200910156617.1 discloses an artificial marble unsaturated polyester resin and a preparation method thereof, although the resin obtained by adding isophthalic acid to the raw material has better hydrolytic stability, higher hardness, higher strength, higher thermal decomposition temperature and better chemical resistance than phthalic acid type unsaturated resin; however, the hardness, strong acid corrosion resistance, strong base corrosion resistance and hydrolysis resistance of the unsaturated polyester resins provided by the patent are still to be improved.
In the production process of resin, raw materials are required to be fed into a reaction kettle through a feeding device, and Chinese patent application number 201810074267.3 discloses automatic feeding production equipment of unsaturated polyester resin, which comprises an automatic feeding mechanism, a closed unpacking mechanism, a vacuum suction mechanism and the reaction kettle, wherein the automatic feeding mechanism comprises a bale grabbing manipulator and a conveying belt; although this patent is through adopting closed automatic bale breaking mode, the smell of the produced dust and material when avoiding throwing the material is to the influence of human body and environment, in the production process of resin, need carry out the decompression evacuation to the resin, also need send into reation kettle's inside to partial raw materials after the decompression evacuation, and when reation kettle was in vacuum state, send into reation kettle's inside the air easily when sending into reation kettle's inside to the raw materials through this patent, destroy reation kettle's vacuum state.
In the production process of resin, sampling is required before the pressure reduction and vacuum pumping of the reaction kettle, and sampling is also required after the pressure reduction and vacuum pumping of the reaction kettle, the method for directly sampling from the reaction kettle in the prior art has a plurality of defects, for example, the sampling is easy to scald at high temperature, the sampling valve is easy to mix air into the kettle when the reaction kettle is in vacuum, and the direct sampling has no buffer process, so that the resin is easily sprayed out in large quantity to cause waste; chinese patent application No. 201020274584.9 discloses a sampling device for polyester resin, which comprises a sampling device shell, a stirring component and a reaction component, wherein although the sampling device can sample the polyester resin without opening a reaction chamber, the resin sampled last time is easy to remain in the sampling chamber, so that the sampled material sampled last time pollutes the sampled material, the detection accuracy of the sampled material is reduced, and the chemical properties of the material in a reaction kettle are not easy to know by a worker.
Disclosure of Invention
In view of the above, the present invention aims to provide a modified water-resistant resin and a preparation method thereof, wherein the modified water-resistant resin is prepared by selecting raw materials, optimizing the content of each raw material, and selecting maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol, a catalyst, a polymerization inhibitor and a diluent, wherein the advantages of the raw materials are fully exerted, and the mutual promotion is provided, such that the modified water-resistant resin is superior to the resin in the prior art in terms of Babbitt hardness, strong acid corrosion resistance, strong base corrosion resistance and hydrolysis stability.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the modified waterproof resin is prepared from the following raw materials in parts by weight: 18-21 parts of maleic anhydride, 23-25 parts of isophthalic anhydride, 20-26 parts of neopentyl glycol, 11-15 parts of propylene glycol, 0.2-0.3 part of catalyst, 0.01-0.02 part of polymerization inhibitor and 25-32 parts of diluent.
Preferably, the catalyst is one or more of monobutyltin oxide, dibutyltin oxide and dibutyltin oxide chloride.
Preferably, the polymerization inhibitor is one or more of hydroquinone, tert-butylhydroquinone, p-tert-butylcatechol and copper naphthenate.
Preferably, the diluent is styrene.
A preparation method of modified water-resistant resin adopts a reaction system for resin production to continuously produce and prepare the resin, and comprises the following steps:
1) Weighing the raw materials of the modified water-resistant resin according to the parts by weight;
2) Feeding maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol and a catalyst into a reaction kettle by adopting a first feeding device;
3) Introducing nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, forming a nitrogen atmosphere in the reaction kettle, blowing the first feeding device by the nitrogen, and blowing residual raw materials in the first feeding device into the reaction kettle;
4) Heating the reaction kettle to 205-210 ℃, and carrying out heat preservation stirring reaction for 6-8 h;
5) The vacuum pump and the pressure regulating pipeline are adopted to reduce the internal pressure of the sampling device, so that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, the sampling device is adopted to carry out differential pressure sampling on the materials in the reaction kettle, when the measured acid value of the sampled materials is 75-80mgKOH/g, the vacuum pump and the pressure regulating pipeline are adopted to carry out vacuum pumping on the reaction kettle for 40-110 min, and the vacuum degree of the reaction kettle is less than or equal to-0.08 Mpa.
6) Then cooling the reaction kettle to 165-175 ℃, adding a polymerization inhibitor into the first feeding device, reducing the internal pressure of the first feeding device by using a vacuum pump and a pressure regulating pipe to make the internal pressure of the first feeding device consistent with the internal pressure of the reaction kettle, then feeding the polymerization inhibitor in the first feeding device into the reaction kettle, and carrying out heat preservation stirring reaction for 1.5-2.5 hours;
7) Feeding the diluent into the dilution kettle by adopting a second feeding device, introducing nitrogen into the dilution kettle by adopting a nitrogen filling device, a pressure regulating pipeline and the second feeding device, forming a nitrogen atmosphere in the dilution kettle, blowing the second feeding device by the nitrogen, and blowing the residual diluent in the second feeding device into the dilution kettle;
8) Reducing the internal pressure of the sampling device by adopting a vacuum pump and a pressure regulating pipeline to ensure that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, carrying out differential pressure sampling on the materials in the reaction kettle by adopting the sampling device, and cooling the reaction kettle to 115-125 ℃ when the measured acid value of the sampled materials is 20-25 mgKOH/g;
9) Feeding nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, relieving the vacuum state in the reaction kettle and enabling the internal pressure of the reaction kettle to be greater than the internal pressure of the dilution kettle;
10 Adopting a first material conveying device to convey materials in the reaction kettle to the dilution kettle, and continuously conveying nitrogen into the reaction kettle through the nitrogen filling device, the pressure regulating pipeline and the first feeding device to ensure that the internal pressure of the reaction kettle is always greater than that of the dilution kettle, thereby being beneficial to completely conveying the materials in the reaction kettle to the dilution kettle;
11 Stirring and mixing the materials in the dilution kettle to obtain modified water-resistant resin;
12 The modified water-resistant resin in the dilution kettle is conveyed to a finished product tank by a second conveying device.
Preferably, reaction system for resin production includes reation kettle, with the first feed arrangement of reation kettle's top intercommunication, with the sampling device of one side intercommunication of reation kettle, with the first feeding device of reation kettle's bottom intercommunication, with the dilution cauldron of first feeding device intercommunication, with the second feed arrangement of dilution cauldron's top intercommunication, with the second feeding device of dilution cauldron's bottom intercommunication, with the finished product jar of second feeding device intercommunication, with the pressure control pipeline that reation kettle, first feed arrangement, sampling device, dilution cauldron and second feeding device all communicate, with the nitrogen charging device of pressure control pipeline intercommunication, with the vacuum pump of pressure control pipeline intercommunication.
Preferably, the upper parts of one sides of the reaction kettle and the dilution kettle are respectively provided with an exhaust pipe, and a filter and an exhaust valve are fixedly arranged in the exhaust pipes.
Preferably, the first feeding device comprises a first feeding pipe communicated with the top of the reaction kettle, a first feeding valve arranged inside the first feeding pipe, a feeding buffer bin communicated with the upper end of the first feeding pipe, a second feeding pipe communicated with the top of the feeding buffer bin, a second feeding valve arranged inside the second feeding pipe, and a feeding hopper communicated with the upper end of the second feeding pipe; the pressure regulating pipeline is communicated with the second feeding pipe, and the communication position of the pressure regulating pipeline and the second feeding pipe is positioned between the second feeding valve and the feeding buffer bin.
Further, the interior top of feeding surge bin is middle high, low setting all around, the interior bottom of feeding surge bin is middle low, high setting all around, and this kind of design does benefit to nitrogen gas and sweeps the raw materials that remain in the feeding surge bin to reation kettle.
Furthermore, a pressure sensor is embedded in the inner wall of the feeding buffer bin.
Preferably, the structure of the second feeding device is identical to that of the first feeding device.
Preferably, the sampling device comprises a sampling pipe communicated with the reaction kettle, a sampling valve arranged inside the sampling pipe, a sampling buffer bin communicated with the sampling pipe, a discharge pipe communicated with the bottom of the sampling buffer bin, a discharge valve arranged inside the discharge pipe, a piston positioned inside the sampling buffer bin, and a cylinder arranged at the top of the sampling buffer bin and used for driving the piston to ascend or descend; the pressure regulating pipeline is communicated with the sampling pipe, and the communicating position of the pressure regulating pipeline and the sampling pipe is positioned between the discharge valve and the sampling buffer bin.
Furthermore, the inner bottom of the sampling buffer bin is low in the middle and high in the periphery, and the discharge pipe is communicated with the lowest point of the sampling buffer bin; the bottom shape of piston suits with the interior bottom shape of sample surge bin, can discharge the sample material in the sample surge bin to the container completely through cylinder and piston to can avoid the sample material pollution of last time sample material this time, promote the detection accuracy of sample material, be favorable to the staff accuracy to learn the chemical property of the inside material of reation kettle.
And a pressure sensor is embedded in the inner wall of the sampling buffer bin.
Preferably, first feeding device includes the first conveying pipeline with reation kettle intercommunication, sets up the first conveying pipeline valve of the inside of first conveying pipeline, with the high viscosity pump of first conveying pipeline intercommunication, with the second conveying pipeline of high viscosity pump intercommunication sets up the second conveying pipeline valve of the inside of second conveying pipeline, the one end that high viscosity pump was kept away from to the second conveying pipeline communicates with the top of diluting the cauldron.
Preferably, the structure of the second material conveying device is consistent with that of the first material conveying device.
Preferably, the pressure regulating pipeline includes that both ends seal the person in charge that sets up, sets up be responsible for on, and with the first branch pipe of reation kettle intercommunication, set up be responsible for on, and with the second branch pipe of first feed arrangement intercommunication sets up be in on the branch pipe and with the third branch pipe of sampling device intercommunication sets up on the branch pipe and with the fourth branch pipe of dilution cauldron intercommunication sets up on the branch pipe and with the fifth branch pipe of second feed arrangement intercommunication sets up be responsible for on, and with the sixth branch pipe of nitrogen charging device intercommunication sets up be responsible for on, and with the seventh branch pipe of vacuum pump intercommunication.
Furthermore, a filter and a regulating valve are fixedly arranged in the first branch pipe, the second branch pipe, the third branch pipe, the fourth branch pipe, the fifth branch pipe, the sixth branch pipe and the seventh branch pipe.
Preferably, the nitrogen charging device comprises an air pump communicated with the pressure regulating pipeline, an air conveying pipe communicated with the air pump, an air conveying valve arranged inside the air conveying pipe, and a nitrogen storage tank communicated with the air conveying pipe.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1) The raw materials of the modified water-resistant resin are selected from maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol, a catalyst, a polymerization inhibitor and a diluent, the content of each raw material is optimized, the respective advantages of the raw materials are fully exerted, and mutual promotion is realized, so that the modified water-resistant resin with superior Babbitt hardness, strong acid corrosion resistance, strong alkali corrosion resistance and hydrolysis stability to the resin in the prior art is prepared.
2) The modified water-resistant resin is produced by adopting a special reaction system for resin production, the reaction system for resin production has a relatively simple integral structure, is convenient to use, and realizes the continuous production of the modified water-resistant resin.
3) The device comprises a first feeding pipe, a first feeding valve, a feeding buffer bin, a second feeding pipe, a second feeding valve and a feeding hopper; the pressure regulating pipeline is communicated with the second feeding pipe, so that the nitrogen filling device can be fed into the reaction kettle through the paths of the pressure regulating pipeline, the second feeding pipe, the feeding buffer bin and the first feeding pipe, the conventional process of replacing air by using nitrogen can also have a purging effect on the feeding device by using nitrogen in the process of forming a nitrogen atmosphere in the reaction kettle, and the occurrence of residual raw materials in the feeding device is avoided; the vacuum pump can reduce the internal pressure in feeding surge bin through the pressure regulation pipeline for the internal pressure in feeding surge bin is unanimous with reation kettle's internal pressure, and when reation kettle was in vacuum state, need not destroy reation kettle's vacuum state just can send into reation kettle's inside to the raw materials, has realized isobaric feeding.
4) Through the arrangement of a sampling pipe, a sampling valve, a sampling buffer bin, a discharging pipe, a discharging valve, a piston and a cylinder; and make pressure regulation pipeline and sampling tube intercommunication, the vacuum pump can make the internal pressure of sample surge bin be less than reation kettle's internal pressure through the pressure regulation pipeline, make in the reation kettle material can be by pressure differential propulsion sample surge bin in, realize the differential pressure sample of the inside material of reation kettle, and fill nitrogen device and can sweep the sampling tube through the pressure regulation pipeline, avoid the material to remain in the sampling tube, and can also discharge the sample material in the sample surge bin to the container completely through cylinder and piston, thereby can avoid the sample material pollution of the last time sample material this time, promote the detection accuracy of sample material.
Drawings
FIG. 1 is a schematic view of the structure of a reaction system for resin production according to the present invention;
FIG. 2 is a schematic view of a portion of the structure of FIG. 1;
FIG. 3 is a schematic structural view of the first feeding device of FIG. 1;
fig. 4 is a schematic structural diagram of the sampling device of fig. 1.
Reference numerals: the reactor comprises a reaction kettle 1, a first feeding device 2, a sampling device 3, a first feeding device 4, a dilution kettle 5, a second feeding device 6, a second feeding device 7, a finished product tank 8, a pressure regulating pipeline 9, a nitrogen charging device 10, a vacuum pump 20, an exhaust pipe 11, a filter 12, an exhaust valve 13, a pressure sensor 14, a regulating valve 15, a first feeding pipe 21, a first feeding valve 22, a feeding buffer bin 23, a second feeding pipe 24, a second feeding valve 25, a feeding hopper 26, a sampling pipe 31, a sampling valve 32, a sampling buffer bin 33, a discharging pipe 34, a discharging valve 35, a piston 36, a cylinder 37, a first feeding pipe 41, a first feeding valve 42, a high viscosity pump 43, a second feeding pipe 44, a second feeding valve 45, a main pipe 91, a first branch pipe 92, a second branch pipe 93, a third branch pipe 94, a fourth branch pipe 95, a fifth branch pipe 96, a sixth branch pipe 97, a seventh branch pipe 98, a gas pipe 101, a gas pipe 102, a gas pump 103 and a nitrogen storage tank 104.
Detailed Description
The following detailed description of the embodiments of the present invention is provided in order to make the technical solution of the present invention easier to understand and understand.
In the present embodiment, it should be understood that the terms "middle", "upper", "lower", "top", "right", "left", "above", "back", "middle", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the present invention, and do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the present embodiment, if the connection or fixing manner between the components is not specifically described, the connection or fixing manner may be a bolt fixing manner, a pin connecting manner, or the like, which is commonly used in the prior art, and therefore, the detailed description thereof is omitted in this embodiment.
Example one
The modified waterproof resin is prepared from the following raw materials in parts by weight: 21 parts of maleic anhydride, 23 parts of isophthalic anhydride, 20 parts of neopentyl glycol, 11 parts of propylene glycol, 0.2 part of catalyst, 0.01 part of polymerization inhibitor and 32 parts of diluent.
In this embodiment, the preparation method of the modified water-resistant resin adopts a reaction system for resin production to continuously produce and prepare the resin, and comprises the following steps:
1) Weighing the raw materials of the modified water-resistant resin according to the parts by weight;
2) Feeding maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol and a catalyst into a reaction kettle by adopting a first feeding device;
3) Introducing nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, forming a nitrogen atmosphere in the reaction kettle, simultaneously purging the first feeding device by the nitrogen, and blowing residual raw materials in the first feeding device into the reaction kettle;
4) Heating the reaction kettle to 205-210 ℃, and carrying out heat preservation and stirring reaction for 6-8 h;
5) Reducing the internal pressure of the sampling device by using a vacuum pump and a pressure regulating pipeline to ensure that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, carrying out differential pressure sampling on the materials in the reaction kettle by using the sampling device, and carrying out vacuum pumping on the reaction kettle for 40-110 min by using the vacuum pump and the pressure regulating pipeline when the measured acid value of the sampled materials is 75-80 mgKOH/g;
6) Then cooling the reaction kettle to 165-175 ℃, adding a polymerization inhibitor into the first feeding device, reducing the internal pressure of the first feeding device by using a vacuum pump and a pressure regulating pipe to make the internal pressure of the first feeding device consistent with the internal pressure of the reaction kettle, then feeding the polymerization inhibitor in the first feeding device into the reaction kettle, and carrying out heat preservation stirring reaction for 1.5-2.5 hours;
7) Feeding the diluent into the diluting kettle by using a second feeding device, introducing nitrogen into the diluting kettle by using a nitrogen filling device, a pressure regulating pipeline and the second feeding device, forming a nitrogen atmosphere in the diluting kettle, purging the second feeding device by using the nitrogen in the process, and blowing the residual diluent in the second feeding device into the diluting kettle;
8) Reducing the internal pressure of the sampling device by using a vacuum pump and a pressure regulating pipeline to ensure that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, carrying out differential pressure sampling on the materials in the reaction kettle by using the sampling device, and cooling the reaction kettle to 115-125 ℃ when the measured acid value of the sampled materials is 20-25 mgKOH/g;
9) Feeding nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, relieving the vacuum state in the reaction kettle and enabling the internal pressure of the reaction kettle to be greater than the internal pressure of the dilution kettle;
10 Adopting a first material conveying device to convey materials in the reaction kettle to the dilution kettle, and continuously conveying nitrogen into the reaction kettle through a nitrogen filling device, a pressure regulating pipeline and a first feeding device to ensure that the internal pressure of the reaction kettle is consistently greater than that of the dilution kettle;
11 ) stirring and mixing the materials in the dilution kettle to prepare the modified water-resistant resin;
12 The modified water-resistant resin in the dilution kettle is conveyed to a finished product tank by a second conveying device.
As shown in fig. 1, the reaction system for producing resin includes a reaction kettle 1, a first feeding device 2 communicated with the top of the reaction kettle 1, a sampling device 3 communicated with the lower portion of one side of the reaction kettle 1, a first feeding device 4 communicated with the bottom of the reaction kettle 1, a dilution kettle 5 communicated with the first feeding device 4, a second feeding device 6 communicated with the top of the dilution kettle 5, a second feeding device 7 communicated with the bottom of the dilution kettle 5, a product tank 8 communicated with the second feeding device 7, a pressure adjusting pipeline 9 communicated with the reaction kettle 1, the first feeding device 2, the sampling device 3, the dilution kettle 5 and the second feeding device 6, a nitrogen filling device 10 communicated with the pressure adjusting pipeline 9, and a vacuum pump 20 communicated with the pressure adjusting pipeline 9.
As shown in fig. 2, exhaust pipes 11 are provided at upper portions of one sides of the reaction vessel 1 and the dilution vessel 5, and a filter 12 and an exhaust valve 13 are fixedly installed inside the exhaust pipes 11. First feeding device 4 includes 41 with the first conveying pipeline of reation kettle 1 intercommunication, sets up the first conveying valve 42 of the inside of first conveying pipeline 41, with the high viscosity pump 43 of 41 intercommunications of first conveying pipeline, with the second conveying pipeline 44 of high viscosity pump 43 intercommunication sets up the second conveying valve 45 of the inside of second conveying pipeline 44, the one end that high viscosity pump 43 was kept away from to second conveying pipeline 44 and the top intercommunication of diluting cauldron 5. The structure of the second feeding device 7 is the same as that of the first feeding device 4.
Pressure regulation pipeline 9 includes that both ends seal the person in charge 91 that sets up, sets up be responsible for 91 on and with the first branch pipe 92 of reation kettle 1 intercommunication, set up be responsible for 91 on and with the second branch pipe 93 of first feed arrangement 2 intercommunication sets up be responsible for on the branch pipe 91 and with the third branch pipe 94 of sampling device 3 intercommunication sets up on the branch pipe 91 and with the fourth branch pipe 95 of diluting cauldron 5 intercommunication sets up be responsible for on 91 and with the fifth branch pipe 96 of second feed arrangement 6 intercommunication, set up be responsible for 91 on and with fill the sixth branch pipe 97 of nitrogen device 10 intercommunication, set up be responsible for 91 on and with the seventh branch pipe 98 of vacuum pump 20 intercommunication. The filter 12 and the regulating valve 15 are fixedly arranged in the first branch pipe 92, the second branch pipe 93, the third branch pipe 94, the fourth branch pipe 95, the fifth branch pipe 96, the sixth branch pipe 97 and the seventh branch pipe 98. The nitrogen charging device 10 comprises an air pump 101 communicated with the pressure regulating pipeline 9, an air pipe 102 communicated with the air pump 101, an air delivery valve 103 arranged inside the air pipe 102, and a nitrogen storage tank 104 communicated with the air pipe 102.
As shown in fig. 3, the first feeding device 2 includes a first feeding pipe 21 communicating with the top of the reaction vessel 1, a first feeding valve 22 disposed inside the first feeding pipe 21, a feeding buffer bin 23 communicating with the upper end of the first feeding pipe 21, a second feeding pipe 24 communicating with the top of the feeding buffer bin 23, a second feeding valve 25 disposed inside the second feeding pipe 24, a feeding hopper 26 communicating with the upper end of the second feeding pipe 24; the pressure regulating line 9 is communicated with the second feeding pipe 24, and the communication position of the pressure regulating line 9 and the second feeding pipe 24 is positioned between the second feeding valve 26 and the feeding buffer bin 23. The interior top of feeding surge bin 23 is middle high, low setting all around, the interior bottom of feeding surge bin 23 is middle low, high setting all around, and this kind of design does benefit to nitrogen gas and sweeps to reation kettle 1 to the raw materials that remain in the feeding surge bin 23. The inner wall of the feeding buffer bin 23 is embedded with a pressure sensor 14. The structure of the second feeding device 6 is identical to that of the first feeding device 2.
As shown in fig. 4, the sampling device 3 includes a sampling pipe 31 communicated with the reaction vessel 1, a sampling valve 32 disposed inside the sampling pipe 31, a sampling buffer bin 33 communicated with the sampling pipe 31, a discharge pipe 34 communicated with the bottom of the sampling buffer bin 33, a discharge valve 35 disposed inside the discharge pipe 34, a piston 36 located inside the sampling buffer bin 33, and a cylinder 37 disposed at the top of the sampling buffer bin 33 and configured to drive the piston 36 to ascend or descend; the pressure regulating pipeline 9 is communicated with the sampling pipe 31, and the communication position of the pressure regulating pipeline 9 and the sampling pipe 31 is positioned between the discharge valve 35 and the sampling buffer bin 33. The inner bottom of the sampling buffer bin 33 is low in the middle and high in the periphery, and the discharge pipe 34 is communicated with the lowest point of the sampling buffer bin 33; the bottom shape of piston 36 suits with the interior bottom shape of sample surge bin 33, can discharge the sample material in the sample surge bin 33 to the container completely through cylinder 37 and piston 36 to can avoid the sample material pollution of last time sample material this time, promote the detection accuracy of sample material. The inner wall of the sampling buffer bin 33 is embedded with a pressure sensor 14. Adopt the sampling process of sampling device 3 to reation kettle 1's inside material, close sampling valve 32, bleeder valve 35, open the governing valve of third branch pipe, the governing valve and the vacuum pump 20 of seventh branch pipe, adopt vacuum pump 20 and pressure regulating pipeline 9 to reduce the internal pressure of sample surge bin 33, make the internal pressure of sample surge bin be less than reation kettle 1's internal pressure, close the governing valve of seventh branch pipe 98 again, the governing valve and the vacuum pump 20 of third branch pipe 94, open sampling valve 32, reation kettle 1's inside material is inhaled to sample surge bin 33 under the effect of pressure differential, accomplish differential pressure sampling, close sampling valve 32 again, put the container that is used for holding the sample material to the exit of discharging pipe 34 again, open bleeder valve 35, and start cylinder 37, cylinder 37 drives piston 36 and discharges the sample material in the sample surge bin 33 to the container.
Example two
The modified waterproof resin is prepared from the following raw materials in parts by weight: 19 parts of maleic anhydride, 24 parts of isophthalic anhydride, 24 parts of neopentyl glycol, 12 parts of propylene glycol, 0.3 part of catalyst, 0.02 part of polymerization inhibitor and 29 parts of diluent.
The preparation method of the second embodiment is the same as that of the first embodiment.
EXAMPLE III
The modified waterproof resin is prepared from the following raw materials in parts by weight: 18 parts of maleic anhydride, 25 parts of isophthalic anhydride, 26 parts of neopentyl glycol, 15 parts of propylene glycol, 0.3 part of catalyst, 0.02 part of polymerization inhibitor and 25 parts of diluent.
The preparation method of the third embodiment is the same as that of the first embodiment.
Comparative example
The resin is prepared according to the technical scheme of the unsaturated polyester resin for the artificial marble and the preparation method thereof disclosed in Chinese patent application No. 200910156617.1.
The unsaturated polyester resin for artificial marble is prepared by the following raw materials in parts by weight: propylene glycol 14%, neopentyl glycol 10%, glycerol 4%, isophthalic acid 20%, phthalic anhydride 14%, maleic anhydride 11% and styrene 27%.
The raw materials of propylene glycol, neopentyl glycol, glycerol and isophthalic acid are added into a reaction kettle for polycondensation reaction at one time, nitrogen protection is provided, and the reaction temperature is controlled to be 195-205 ℃ and the acid value reaches 40 +/-5 mgKOH/g after 12 hours of polycondensation; cooling to 160 ℃, adding phthalic anhydride and maleic anhydride into synthesis equipment, carrying out polycondensation for 7h, controlling the reaction temperature to be 195-205 ℃, controlling the acid value to be 60 +/-5 mgKOH/g, carrying out vacuum treatment under reduced pressure, keeping the vacuum degree to be more than or equal to 0.092Mpa, vacuumizing for 2h-4h, and keeping the material temperature to be 198-202 ℃ until the acid value is 25-35mgKOH/g; cooling to 190 deg.C, adding 0.005% mixture of benzenetriol and hydroquinone, stirring, cooling to 100-120 deg.C, adding styrene, stirring, cooling to room temperature, and making into unsaturated polyester resin.
Specific parameter settings are provided according to the technical indexes of the unsaturated polyester resin casting body for the artificial stone recorded in DB 35/T1826-2019, and are specifically shown in the following table 1;
TABLE 1
The data obtained by testing the experimental products prepared in the first, second, third, fourth and comparative examples are shown in the following table 2:
TABLE 2
As can be seen from tables 1 and 2, the modified water-resistant resin of the present invention satisfies the criteria described in DB 35/T1826-2019 in terms of Barcol hardness, flexural strength, tensile strength, elongation at break, flexural modulus of elasticity, impact strength and heat distortion temperature, and is superior to the comparative examples in terms of Babbitt hardness, resistance to strong acid corrosion, resistance to strong base corrosion and hydrolytic stability.
Of course, the above is only a typical example of the present invention, and besides, the present invention may have other embodiments, and all technical solutions formed by using equivalent substitutions or equivalent transformations fall within the scope of the present invention.
Claims (1)
1. The preparation method of the modified water-resistant resin is characterized by adopting a reaction system for resin production to continuously produce and prepare the resin, and comprises the following steps:
1) Weighing the raw materials of the modified water-resistant resin according to parts by weight, and preparing the modified water-resistant resin from the following raw materials in parts by weight: 18-21 parts of maleic anhydride, 23-25 parts of isophthalic anhydride, 20-26 parts of neopentyl glycol, 11-15 parts of propylene glycol, 0.2-0.3 part of catalyst, 0.01-0.02 part of polymerization inhibitor and 25-32 parts of diluent, wherein the catalyst is one or more of monobutyl tin oxide, dibutyl tin oxide and dibutyl tin oxide chloride;
2) Feeding maleic anhydride, isophthalic anhydride, neopentyl glycol, propylene glycol and a catalyst into a reaction kettle by adopting a first feeding device;
3) Introducing nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, forming a nitrogen atmosphere in the reaction kettle, simultaneously purging the first feeding device by the nitrogen, and blowing residual raw materials in the first feeding device into the reaction kettle;
4) Heating the reaction kettle to 205-210 ℃, and carrying out heat preservation stirring reaction for 6-8 h;
5) Reducing the internal pressure of the sampling device by using a vacuum pump and a pressure regulating pipeline to ensure that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, carrying out differential pressure sampling on the materials in the reaction kettle by using the sampling device, and carrying out vacuum pumping on the reaction kettle for 40-110 min by using the vacuum pump and the pressure regulating pipeline when the measured acid value of the sampled materials is 75-80 mgKOH/g;
6) Then cooling the reaction kettle to 165-175 ℃, adding a polymerization inhibitor into the first feeding device, reducing the internal pressure of the first feeding device by adopting a vacuum pump and a pressure regulating pipe to make the internal pressure of the first feeding device consistent with the internal pressure of the reaction kettle, then feeding the polymerization inhibitor in the first feeding device into the reaction kettle, and carrying out heat preservation stirring reaction for 1.5-2.5 hours;
7) Feeding the diluent into the diluting kettle by adopting a second feeding device, introducing nitrogen into the diluting kettle by adopting a nitrogen filling device, a pressure regulating pipeline and the second feeding device, forming a nitrogen atmosphere in the diluting kettle, simultaneously purging the second feeding device by using the nitrogen, and blowing the residual diluent in the second feeding device into the diluting kettle;
8) Reducing the internal pressure of the sampling device by using a vacuum pump and a pressure regulating pipeline to ensure that the internal pressure of the sampling device is less than the internal pressure of the reaction kettle, carrying out differential pressure sampling on the materials in the reaction kettle by using the sampling device, and cooling the reaction kettle to 115-125 ℃ when the measured acid value of the sampled materials is 20-25 mgKOH/g;
9) Feeding nitrogen into the reaction kettle by adopting a nitrogen filling device, a pressure regulating pipeline and a first feeding device, relieving the vacuum state in the reaction kettle and enabling the internal pressure of the reaction kettle to be greater than the internal pressure of the dilution kettle;
10 Adopting a first material conveying device to convey materials in the reaction kettle into the dilution kettle, and meanwhile, continuously conveying nitrogen into the reaction kettle through a nitrogen filling device, a pressure regulating pipeline and a first feeding device so as to enable the internal pressure of the reaction kettle to be always greater than that of the dilution kettle;
11 ) stirring and mixing the materials in the dilution kettle to prepare the modified water-resistant resin;
12 Adopting a second material conveying device to convey the modified waterproof resin in the dilution kettle to a finished product tank;
the reaction system for resin production comprises a reaction kettle, a first feeding device communicated with the top of the reaction kettle, a sampling device communicated with one side of the reaction kettle, a first material conveying device communicated with the bottom of the reaction kettle, a dilution kettle communicated with the first material conveying device, a second feeding device communicated with the top of the dilution kettle, a second material conveying device communicated with the bottom of the dilution kettle, a finished product tank communicated with the second material conveying device, a pressure regulating pipeline communicated with the reaction kettle, the first feeding device, the sampling device, the dilution kettle and the second feeding device, a nitrogen filling device communicated with the pressure regulating pipeline, and a vacuum pump communicated with the pressure regulating pipeline, wherein the first feeding device comprises a first feeding pipe communicated with the top of the reaction kettle, a first feeding valve arranged inside the first feeding pipe, a feeding buffer bin communicated with the upper end of the first feeding pipe, a second feeding pipe communicated with the top of the feeding buffer bin, a second feeding pipe arranged inside the second feeding pipe, and the upper end of the second feeding hopper; the sampling device comprises a sampling pipe communicated with the reaction kettle, a sampling valve arranged inside the sampling pipe, a sampling buffer bin communicated with the sampling pipe, a discharging pipe communicated with the bottom of the sampling buffer bin, a discharging valve arranged inside the discharging pipe, a piston arranged inside the sampling buffer bin, and a cylinder which is arranged at the top of the sampling buffer bin and is used for driving the piston to ascend or descend; pressure regulation pipeline and sampling tube intercommunication, just the intercommunication department of pressure regulation pipeline and sampling tube is located between bleeder valve and the sample surge bin, first feeding device includes the first conveying pipeline with the reation kettle intercommunication, sets up the first conveying pipeline of the inside of first conveying pipeline, with the high viscosity pump of first conveying pipeline intercommunication, with the second conveying pipeline of high viscosity pump intercommunication sets up the second conveying pipeline of the inside of second conveying pipeline, the one end that high viscosity pump was kept away from to the second conveying pipeline and the top intercommunication of diluting the cauldron, the pressure regulation pipeline includes that both ends seal the setting, set up be responsible for, and with the first branch pipe of reation kettle intercommunication, set up be responsible for, and with the second branch pipe of first feeding device intercommunication, set up be in on the branch pipe and with the third branch pipe of sampling device intercommunication, set up branch pipe on the diluting the cauldron, and with the fourth branch pipe of diluting the cauldron intercommunication, set up on the branch pipe and with the fifth branch pipe of second feeding device intercommunication and the nitrogen gas pump intercommunication is in the nitrogen filling device and the nitrogen filling device is equipped with the fourth branch pipe, the nitrogen filling device and the nitrogen filling device is equipped with the fourth branch pipe intercommunication.
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| US4031289A (en) * | 1976-05-11 | 1977-06-21 | The Burns & Russell Company Of Baltimore City | Stain resistant polyester-coated block |
| CN101735405B (en) * | 2009-12-29 | 2011-08-03 | 浙江天和树脂有限公司 | Imitation marble unsaturated polyester resin and preparation method thereof |
| CN201773016U (en) * | 2010-07-29 | 2011-03-23 | 常州华科树脂有限公司 | Polyester resin sampling device |
| CN102627740A (en) * | 2012-03-21 | 2012-08-08 | 常州华科树脂有限公司 | Low styrene volatilization unsaturated polyester gel coat resin and preparation method thereof |
| CN206248405U (en) * | 2016-12-15 | 2017-06-13 | 安庆市索隆新材料有限公司 | A kind of polyester synthesis reactor sealed sampling device |
| CN108499487A (en) * | 2018-03-19 | 2018-09-07 | 江苏大力士投资有限公司 | A kind of production system and its production method of unsaturated-resin |
| CN108997567A (en) * | 2018-09-11 | 2018-12-14 | 惠州市固德尔合成材料有限公司 | A kind of unsaturated-resin material and preparation method thereof suitable for sanitary ware manufacture |
| CN210166178U (en) * | 2019-06-13 | 2020-03-20 | 南通星辰合成材料有限公司 | Reaction kettle vacuum sampling device |
| CN110658029A (en) * | 2019-11-20 | 2020-01-07 | 郎蕾 | Differential pressure type polyester resin sampling device |
| CN112321199A (en) * | 2020-11-04 | 2021-02-05 | 广州戈兰迪新材料股份有限公司 | Iodophor permeation resistant antibacterial artificial stone and preparation method thereof |
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Denomination of invention: A modified water-resistant resin and its preparation method Granted publication date: 20221209 Pledgee: Wengyuan County sub branch of Agricultural Bank of China Ltd. Pledgor: Guangdong Huiquan Lianjun Chemical Industry Co.,Ltd. Registration number: Y2024980008701 |