CN114394888A - D-33 diol monomer and preparation method thereof - Google Patents
D-33 diol monomer and preparation method thereof Download PDFInfo
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- CN114394888A CN114394888A CN202111396971.9A CN202111396971A CN114394888A CN 114394888 A CN114394888 A CN 114394888A CN 202111396971 A CN202111396971 A CN 202111396971A CN 114394888 A CN114394888 A CN 114394888A
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- 239000000178 monomer Substances 0.000 title claims abstract description 35
- 150000002009 diols Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 82
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 33
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 33
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims description 86
- 238000004821 distillation Methods 0.000 claims description 35
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 21
- 239000011343 solid material Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 16
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 15
- 238000005070 sampling Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011344 liquid material Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 23
- 235000011007 phosphoric acid Nutrition 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 239000004645 polyester resin Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- LPIQUOYDBNQMRZ-UHFFFAOYSA-N cyclopentene Chemical compound C1CC=CC1 LPIQUOYDBNQMRZ-UHFFFAOYSA-N 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- WECJUPODCKXNQK-UHFFFAOYSA-N 1-methoxy-4-[(4-methoxyphenyl)methyl]benzene Chemical compound C1=CC(OC)=CC=C1CC1=CC=C(OC)C=C1 WECJUPODCKXNQK-UHFFFAOYSA-N 0.000 description 1
- HBAQYPYDRFILMT-UHFFFAOYSA-N 8-[3-(1-cyclopropylpyrazol-4-yl)-1H-pyrazolo[4,3-d]pyrimidin-5-yl]-3-methyl-3,8-diazabicyclo[3.2.1]octan-2-one Chemical class C1(CC1)N1N=CC(=C1)C1=NNC2=C1N=C(N=C2)N1C2C(N(CC1CC2)C)=O HBAQYPYDRFILMT-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C43/00—Ethers; Compounds having groups, groups or groups
- C07C43/02—Ethers
- C07C43/20—Ethers having an ether-oxygen atom bound to a carbon atom of a six-membered aromatic ring
- C07C43/23—Ethers having an ether-oxygen atom bound to a carbon atom of a six-membered aromatic ring containing hydroxy or O-metal groups
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of chemical material preparation, in particular to a D-33 diol monomer and a preparation method thereof. A D-33 diol monomer comprises the following raw materials in parts by weight: 28-33 parts of bisphenol A, 19-22 parts of propylene oxide, 0.4-0.5 part of sodium hydroxide, 0.4-0.5 part of phosphoric acid and 7-8 parts of water. The D-33 diol monomer prepared by the preparation method of the D-33 diol monomer has high purity and good quality by selecting proper raw materials and reasonable proportion, and meanwhile, the preparation process is simple and the production efficiency is high.
Description
Technical Field
The invention relates to the field of chemical material preparation, in particular to a D-33 diol monomer and a preparation method thereof.
Background
D-33 diol monomer, chemical name: 4.4- (B-B' -dihydroxydipropoxyphenyl) 2.2-propane. The molecular formula is as follows: C12H28O4, molecular weight: 344.43, light yellow transparent viscous liquid with hydroxyl value of 6-9. The polyester resin has good thermal stability, is not easy to decompose, is nontoxic and non-corrosive, is a main raw material for synthesizing chemical corrosion resistant polyester resin, and is especially an essential raw material for preparing alkali corrosion resistant polyester resin. The traditional preparation process of the D-33 diol monomer is complex and has low production efficiency, and the produced D-33 diol monomer has low purity and poor quality.
Disclosure of Invention
The invention provides a D-33 diol monomer and a preparation method thereof.
A D-33 diol monomer comprises the following raw materials in parts by weight: 28-33 parts of bisphenol A, 19-22 parts of propylene oxide, 0.4-0.5 part of sodium hydroxide, 0.4-0.5 part of phosphoric acid and 7-8 parts of water.
Bisphenol A, also called BPA, is an organic compound with the molecular formula of C15H16O2, is one of the most widely used industrial compounds in the world, and is mainly used for producing various high polymer materials such as polycarbonate, epoxy resin, polysulfone resin, polyphenylene oxide resin, unsaturated polyester resin and the like. And can also be used for producing fine chemical products such as plasticizers, flame retardants, antioxidants, heat stabilizers, rubber antioxidants, pesticides, coatings and the like.
Propylene oxide, also known as propylene oxide, methyl ethylene oxide, 1, 2-propylene oxide, of the formula C3H6O, is a very important organic compound starting material, second only to polypropylene and acrylonitrile, the third largest propylene derivative. Propylene oxide is a colorless ether-flavored liquid, has low boiling point, is inflammable and chiral, and the industrial product is generally a racemic mixture of two enantiomers. Mixing with water, ethanol and diethyl ether. Form binary azeotropic mixtures with pentane, pentene, cyclopentane, cyclopentene, dichloromethane.
Sodium hydroxide, an inorganic compound, NaOH, also known as caustic soda, solid caustic, caustic soda. The sodium hydroxide has strong basicity and strong corrosivity, can be used as an acid neutralizing agent, a complex masking agent, a precipitating agent, a precipitation masking agent, a color developing agent, a saponifying agent, a peeling agent, a detergent and the like, and has wide application. Sodium hydroxide has strong basicity and strong hygroscopicity. Is easy to dissolve in water, releases heat when dissolved, and the water solution is alkaline and has greasy feeling; has strong corrosivity, and has corrosive effect on fiber, skin, glass, ceramic, etc. React with metal aluminum and zinc, nonmetal boron and silicon, etc. to release hydrogen; disproportionation reaction with halogen such as chlorine, bromine, iodine, etc.; neutralizing with acid to generate salt and water.
Phosphoric acid, a common inorganic acid, is a medium strong acid, has a chemical formula of H3PO4, is not easy to volatilize and decompose, and has almost no oxidation. The acid is a ternary weak acid, and the acidity of the acid is weaker than that of hydrochloric acid, sulfuric acid and nitric acid and stronger than that of acetic acid and boric acid.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle, sampling and measuring a hydroxyl value, adding phosphoric acid from a feed inlet of the reaction kettle for neutralization when the hydroxyl value is more than 8.5, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 110-120 ℃, distilling for 10-12h, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 glycol monomer.
Further, in the seventh step, a vertical condenser is adopted to cool the reaction kettle.
Further, in the ninth step, sampling is carried out during the distillation process to determine the content, and when the content of the solid material is more than 95%, the distillation is completed.
In conclusion, the invention has the following beneficial effects:
the D-33 diol monomer prepared by the preparation method of the D-33 diol monomer has high purity and good quality by selecting proper raw materials and reasonable proportion, and meanwhile, the preparation process is simple and the production efficiency is high.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A D-33 diol monomer comprises the following raw materials in parts by weight: 28 parts of bisphenol A, 19 parts of propylene oxide, 0.4 part of sodium hydroxide, 0.4 part of phosphoric acid and 7 parts of water.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle by adopting a vertical condenser, sampling and measuring a hydroxyl value, wherein the measured hydroxyl value is equal to 8.8, adding phosphoric acid from a feeding port of the reaction kettle for neutralization, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 110 ℃, distilling for 10 hours, sampling to determine that the content of the solid material is equal to 96.3%, completing distillation, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 diol monomer.
Example two
A D-33 diol monomer comprises the following raw materials in parts by weight: 30 parts of bisphenol A, 20 parts of propylene oxide, 0.42 part of sodium hydroxide, 0.42 part of phosphoric acid and 7.25 parts of water.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle by adopting a vertical condenser, sampling and measuring a hydroxyl value, wherein the measured hydroxyl value is equal to 8.6, adding phosphoric acid from a feeding port of the reaction kettle for neutralization, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 115 ℃ for distillation, performing distillation for 11 hours, sampling to determine that the content of the solid material is equal to 97.1%, completing distillation, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 diol monomer.
EXAMPLE III
A D-33 diol monomer comprises the following raw materials in parts by weight: 33 parts of bisphenol A, 21 parts of propylene oxide, 0.5 part of sodium hydroxide, 0.48 part of phosphoric acid and 8 parts of water.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle by adopting a vertical condenser, sampling and measuring a hydroxyl value, wherein the measured hydroxyl value is equal to 8.9, adding phosphoric acid from a feeding port of the reaction kettle for neutralization, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 120 ℃ for distillation for 10.5 hours, sampling to determine that the content of the solid material is equal to 96.6%, completing distillation, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 diol monomer.
Example four
A D-33 diol monomer comprises the following raw materials in parts by weight: 32 parts of bisphenol A, 22 parts of propylene oxide, 0.45 part of sodium hydroxide, 0.5 part of phosphoric acid and 7.55 parts of water.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle by adopting a vertical condenser, sampling and measuring a hydroxyl value, wherein the measured hydroxyl value is equal to 8.7, adding phosphoric acid from a feeding port of the reaction kettle for neutralization, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 113 ℃ for distillation, distilling for 11.5 hours, sampling to determine that the content of the solid material is equal to 95.9%, completing distillation, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 diol monomer.
EXAMPLE five
A D-33 diol monomer comprises the following raw materials in parts by weight: 33 parts of bisphenol A, 22 parts of propylene oxide, 0.5 part of sodium hydroxide, 0.5 part of phosphoric acid and 8 parts of water.
A method for preparing a D-33 diol monomer, comprising the steps of:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle by adopting a vertical condenser, sampling and measuring a hydroxyl value, wherein the measured hydroxyl value is equal to 8.8, adding phosphoric acid from a feeding port of the reaction kettle for neutralization, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 120 ℃ for distillation for 12 hours, sampling to determine that the content of the solid material is equal to 97.4%, completing distillation, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 diol monomer.
In summary, the present invention is not limited to the above-described embodiments. Numerous changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention. The protection scope of the present invention shall be subject to the claims of the present invention.
Claims (4)
1. The D-33 diol monomer is characterized by comprising the following raw materials in parts by weight: 28-33 parts of bisphenol A, 19-22 parts of propylene oxide, 0.4-0.5 part of sodium hydroxide, 0.4-0.5 part of phosphoric acid and 7-8 parts of water.
2. A method for preparing a D-33 diol monomer, which is characterized by comprising the following steps:
the method comprises the following steps: pouring sodium hydroxide into a semi-sealed feeding tank, sucking the sodium hydroxide into a reaction kettle through a pipeline, and then adding water into the reaction kettle;
step two: adding bisphenol A into a reaction kettle through a feeding tank;
step three: adding propylene oxide from a feed inlet of the reaction kettle;
step four: heating the reaction kettle to 40 ℃, and stirring simultaneously to uniformly mix the raw materials;
step five: heating the reaction kettle to 60 ℃, and preserving heat for 6 hours;
step six: heating the reaction kettle to 80 ℃, and preserving heat for 4 hours;
step seven: cooling the reaction kettle, sampling and measuring a hydroxyl value, adding phosphoric acid from a feed inlet of the reaction kettle for neutralization when the hydroxyl value is more than 8.5, and stopping reaction;
step eight: standing the neutralized mixed solution in a reaction kettle for 90min for solid-liquid separation, wherein the upper layer is a liquid material, and the lower layer is a solid material;
step nine: and (3) allowing the solid material on the lower layer to flow into a distillation kettle through a pipeline on the bottom layer of the reaction kettle, heating the distillation kettle to 110-120 ℃, distilling for 10-12h, cooling the distillation kettle to 80 ℃, and finally cooling at normal temperature to obtain the solid D-33 glycol monomer.
3. The method according to claim 2, wherein in the seventh step, the reaction kettle is cooled by a vertical condenser.
4. The process for producing a D-33 diol monomer according to claim 3, wherein in the ninth step, a sample is taken during the distillation to determine the content, and the distillation is completed when the solid material content is more than 95%.
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