CN111620779A - Dibutyl phthalate production process capable of preventing crystallization in esterification kettle - Google Patents
Dibutyl phthalate production process capable of preventing crystallization in esterification kettle Download PDFInfo
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- CN111620779A CN111620779A CN202010509974.8A CN202010509974A CN111620779A CN 111620779 A CN111620779 A CN 111620779A CN 202010509974 A CN202010509974 A CN 202010509974A CN 111620779 A CN111620779 A CN 111620779A
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- esterification
- alcohol
- kettle
- esterification kettle
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 108
- 230000032050 esterification Effects 0.000 title claims abstract description 94
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002425 crystallisation Methods 0.000 title claims abstract description 16
- 230000008025 crystallization Effects 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000002351 wastewater Substances 0.000 claims abstract description 16
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- IVLRWAWNKKMBFT-UHFFFAOYSA-N 2-benzofuran-1,3-dione;naphthalene Chemical compound C1=CC=CC2=CC=CC=C21.C1=CC=C2C(=O)OC(=O)C2=C1 IVLRWAWNKKMBFT-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 17
- 229910021529 ammonia Inorganic materials 0.000 description 7
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- 235000011130 ammonium sulphate Nutrition 0.000 description 4
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- URGSMJLDEFDWNX-UHFFFAOYSA-N 1-butylnaphthalene Chemical compound C1=CC=C2C(CCCC)=CC=CC2=C1 URGSMJLDEFDWNX-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000008029 phthalate plasticizer Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production process of dibutyl phthalate for preventing crystallization in an esterification kettle, which comprises the steps of sequentially adding raw materials into the esterification kettle for heating reaction, feeding steam evaporated from the top of the esterification kettle into an esterification tower, condensing the steam by a condenser (1), feeding the condensed steam into an alcohol-water separation tank (1) for alcohol-water separation, adding separated reflux alcohol from the top of the esterification tower, and making the separated reflux alcohol reversely contact with the steam evaporated from the esterification kettle and then flow into the esterification kettle; after the esterification reaction is finished, introducing the product into a neutralization kettle for neutralization, adding the neutralized wastewater from a wastewater tower, then flowing into a reboiler for heating, introducing steam evaporated from the reboiler into a wastewater tower, then condensing the steam by a condenser (2), then entering an alcohol-water separation tank (2) for alcohol-water separation, introducing the separated recovered alcohol into a recovered alcohol replenishing tank, adding the recovered alcohol from the top of the esterification tower, reversely contacting the recovered alcohol with the steam evaporated from the esterification kettle, and then flowing into the esterification kettle for esterification reaction. The production process can obviously reduce the crystal in the esterification kettle and improve the production efficiency.
Description
Technical Field
The invention relates to the technical field of plasticizer production, in particular to a production process of dibutyl phthalate for preventing crystallization in an esterification kettle.
Background
Dibutyl phthalate is a plasticizer product with high plasticizing efficiency and wide application, is mainly used as a main plasticizer for cellulose resins and polyvinyl chloride products, and is particularly suitable for cellulose nitrate resins. Has excellent solubility, decomposability and adhesiveness, and the flexibility and stability of the paint film are also excellent.
When the naphthalene phthalic anhydride raw material is used in the traditional production process, a layer of khaki crystal is often attached to the outer wall of a steam heating pipe in an esterification kettle in the esterification reaction process, so that the heating efficiency of the esterification kettle is seriously influenced, the esterification time is prolonged, and the steam energy consumption is high.
Disclosure of Invention
The invention aims to provide a dibutyl phthalate production process capable of preventing crystallization in an esterification kettle, which can obviously reduce crystals in the esterification kettle and improve the production efficiency.
A production process of dibutyl phthalate for preventing crystallization in an esterification kettle comprises the steps of sequentially adding n-butyl alcohol, naphthalene phthalic anhydride and concentrated sulfuric acid into the esterification kettle for heating reaction, feeding steam evaporated from the top of the esterification kettle into an esterification tower, condensing the steam by a condenser (1), feeding the condensed steam into an alcohol-water separation tank (1) for alcohol-water separation, adding separated reflux alcohol from the top of the esterification tower, and feeding the separated reflux alcohol into the esterification kettle after the reflux alcohol is in reverse contact with the steam evaporated from the esterification kettle; after the esterification reaction is finished, introducing the product into a neutralization kettle for neutralization, adding the neutralized wastewater from a wastewater tower, then flowing into a reboiler for heating, introducing steam evaporated from the reboiler into a wastewater tower, then condensing the steam by a condenser (2), then entering an alcohol-water separation tank (2) for alcohol-water separation, introducing the separated recovered alcohol into a recovered alcohol replenishing tank, adding the recovered alcohol from the top of the esterification tower, reversely contacting the recovered alcohol with the steam evaporated from the esterification kettle, and then flowing into the esterification kettle for esterification reaction.
Further, the reaction temperature of the esterification kettle is 135-150 ℃, and the reaction time is 5.5-6 h.
Further, the temperature of the esterification kettle is increased by heating the esterification kettle by an inner coil pipe.
Further, when the esterification temperature rises to 130 ℃, the recovered alcohol in the recovered alcohol supplementing tank is slowly added to the top of the esterification tower.
Further, sodium hydroxide solution with the concentration of 0.5 percent is selected in the neutralization procedure.
Furthermore, the condenser (1) has a heat exchange area of 70m2The double-tube pass horizontal condenser; the condenser (2) has a heat exchange area of 5m2The double-tube pass horizontal condenser.
The production process of dibutyl phthalate for preventing crystallization in the esterification kettle, disclosed by the invention, has the following beneficial effects:
n-butyl alcohol and naphthalene-process phthalic anhydride are selected as raw materials of the esterification reaction of the dibutyl phthalate plasticizer, concentrated sulfuric acid is selected as a catalyst, the naphthalene-process phthalic anhydride raw materials generally contain a small amount of phthalimide impurities, phthalimide reacts with an alkali solution in a neutralization process to generate ammonia gas, the ammonia gas is dissolved into recovered alcohol (the recovered alcohol generally contains a large amount of water) and added into an esterification kettle to react with the catalyst concentrated sulfuric acid, so that a large amount of ammonium sulfate crystals are generated, the crystals are attached to a heating inner coil pipe, the heating efficiency of the esterification kettle is seriously influenced, the esterification time is prolonged, the steam energy consumption is high, and the heating efficiency is low.
Fresh n-butyl alcohol, naphthalene phthalic anhydride and concentrated sulfuric acid are firstly put into an esterification kettle, the separated recovered alcohol containing ammonia is pumped into a recovered alcohol replenishing tank, when the esterification temperature rises to 130 ℃, the recovered alcohol in the recovered alcohol replenishing tank is slowly added from the top of the esterification tower, so that ammonia gas newly added with ammonia recovered alcohol enters a tower top condenser along with rising hot air flow, and enters an alcohol-water separation tank together with generated water and alcohol, because the ammonia is very soluble in water, the ammonia is discharged out of a system along with water in the middle and lower layers of the alcohol-water separation tank; and the alcohol on the upper layer of the alcohol-water separation tank continuously enters the esterification tower along with the reflux alcohol. The ammonia-containing recovered alcohol slowly placed into the tower top from the recovered alcohol replenishing tank is rectified by the esterification tower, most of the ammonia-containing recovered alcohol enters the esterification kettle, and the alcohol falling into the esterification kettle does not react with sulfuric acid to generate ammonium sulfate crystals because of no ammonia, so that the ammonium sulfate crystals cannot be crystallized on the heating coil. The heating pipe is free from ammonium sulfate and other crystals, so that the heating efficiency of the heating pipe is improved, the aims of shortening the esterification time and saving energy are fulfilled, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of the dibutyl phthalate esterification process flow of the present invention;
FIG. 2 is a schematic diagram of a dibutyl phthalate wastewater treatment process according to the present invention;
description of reference numerals:
1-esterification kettle, 2-esterification tower, 3-condenser (1), 4-alcohol-water separation tank (1), 5-recovered alcohol replenishing tank, 6-waste water tower, 7-reboiler, 8-condenser (2), 9-alcohol-water separation tank (2).
Detailed Description
The process for producing dibutyl phthalate according to the present invention for preventing crystallization in an esterification reactor will be described in detail with reference to the accompanying drawings and examples.
Example 1
The invention relates to a production process of dibutyl phthalate for preventing crystallization in an esterification kettle, which is shown in figures 1 and 2, and comprises the steps of sequentially adding n-butanol, naphthalene-process phthalic anhydride and concentrated sulfuric acid into the esterification kettle 1 for heating reaction, wherein an inner coil pipe is adopted for heating the esterification kettle 1, the reaction temperature of the esterification kettle 1 is 135-150 ℃, and the reaction time is 6 hours. Steam distilled from the top of the esterification kettle 1 enters an esterification tower 2, is condensed by a condenser (1) 3 and then enters an alcohol-water separation tank (1) 4 for alcohol-water separation, and separated reflux alcohol is added from the top of the esterification tower 2 and reversely contacts with the steam distilled from the esterification kettle 1 and then flows into the esterification kettle 1; after the esterification reaction is finished, introducing the product into a neutralization kettle, selecting a sodium hydroxide solution with the concentration of 0.5% for neutralization, adding the neutralized wastewater from a wastewater tower 6, then flowing into a reboiler 7 for heating, condensing steam evaporated by the reboiler 7 after entering the wastewater tower 6 through a condenser (2) 8, then entering an alcohol-water separation tank (2) 9 for alcohol-water separation, introducing the separated recovered alcohol into a recovered alcohol replenishing tank 5, slowly adding the recovered alcohol in the recovered alcohol replenishing tank 5 to the top of the esterification tower 2 when the esterification temperature rises to 130 ℃, and then flowing into the esterification kettle 1 for esterification reaction after reversely contacting with the steam evaporated in the esterification kettle 1.
The condenser (1) has a heat exchange area of 70m2The double-tube pass horizontal condenser; the condenser (2) has a heat exchange area of 5m2The double-tube pass horizontal condenser.
Example 2
The invention relates to a production process of dibutyl phthalate for preventing crystallization in an esterification kettle, which is shown in figures 1 and 2, and comprises the steps of sequentially adding n-butanol, naphthalene-process phthalic anhydride and concentrated sulfuric acid into the esterification kettle 1 for heating reaction, wherein an inner coil pipe is adopted for heating the esterification kettle 1, the reaction temperature of the esterification kettle 1 is 135-150 ℃, and the reaction time is 5.5 hours. Steam distilled from the top of the esterification kettle 1 enters an esterification tower 2, is condensed by a condenser (1) 3 and then enters an alcohol-water separation tank (1) 4 for alcohol-water separation, and separated reflux alcohol is added from the top of the esterification tower 2 and reversely contacts with the steam distilled from the esterification kettle 1 and then flows into the esterification kettle 1; after the esterification reaction is finished, introducing the product into a neutralization kettle, selecting a sodium hydroxide solution with the concentration of 0.5% for neutralization, adding the neutralized wastewater from a wastewater tower 6, then flowing into a reboiler 7 for heating, condensing steam evaporated by the reboiler 7 after entering the wastewater tower 6 through a condenser (2) 8, then entering an alcohol-water separation tank (2) 9 for alcohol-water separation, introducing the separated recovered alcohol into a recovered alcohol replenishing tank 5, slowly adding the recovered alcohol in the recovered alcohol replenishing tank 5 to the top of the esterification tower 2 when the esterification temperature rises to 130 ℃, and then flowing into the esterification kettle 1 for esterification reaction after reversely contacting with the steam evaporated in the esterification kettle 1.
The condenser (1) has a heat exchange area of 70m2The double-tube pass horizontal condenser; the condenser (2) has a heat exchange area of 5m2The double-tube pass horizontal condenser.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A production process of dibutyl phthalate for preventing crystallization in an esterification kettle is characterized in that: sequentially adding n-butyl alcohol, naphthalene phthalic anhydride and concentrated sulfuric acid into an esterification kettle for heating reaction, allowing steam evaporated from the top of the esterification kettle to enter an esterification tower, condensing the steam by a condenser (1), allowing the condensed steam to enter an alcohol-water separation tank (1) for alcohol-water separation, adding separated reflux alcohol from the top of the esterification tower, and allowing the separated reflux alcohol to reversely contact with the steam evaporated from the esterification kettle and then flow into the esterification kettle; after the esterification reaction is finished, introducing the product into a neutralization kettle for neutralization, adding the neutralized wastewater from a wastewater tower, then flowing into a reboiler for heating, introducing steam evaporated from the reboiler into a wastewater tower, then condensing the steam by a condenser (2), then entering an alcohol-water separation tank (2) for alcohol-water separation, introducing the separated recovered alcohol into a recovered alcohol replenishing tank, adding the recovered alcohol from the top of the esterification tower, reversely contacting the recovered alcohol with the steam evaporated from the esterification kettle, and then flowing into the esterification kettle for esterification reaction.
2. The process for producing dibutyl phthalate according to claim 1, wherein the crystallization in the esterification kettle is prevented by: the reaction temperature of the esterification kettle is 135-150 ℃, and the reaction time is 5.5-6 h.
3. The process for producing dibutyl phthalate according to claim 1, wherein the crystallization in the esterification kettle is prevented by: the temperature of the esterification kettle is increased by heating the esterification kettle by an inner coil pipe.
4. The process for producing dibutyl phthalate according to claim 1, wherein the crystallization in the esterification kettle is prevented by: when the esterification temperature rises to 130 ℃, the recovered alcohol in the recovered alcohol replenishing tank is slowly added to the top of the esterification tower.
5. The process for producing dibutyl phthalate according to claim 1, wherein the crystallization in the esterification kettle is prevented by: the neutralization step uses 0.5% sodium hydroxide solution.
6. The process for producing dibutyl phthalate according to claim 1, wherein the crystallization in the esterification kettle is prevented by: the condenser (1) has a heat exchange area of 70m2The double-tube pass horizontal condenser; the condenser (2) has a heat exchange area of 5m2The double-tube pass horizontal condenser.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010509974.8A CN111620779A (en) | 2020-06-08 | 2020-06-08 | Dibutyl phthalate production process capable of preventing crystallization in esterification kettle |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010509974.8A CN111620779A (en) | 2020-06-08 | 2020-06-08 | Dibutyl phthalate production process capable of preventing crystallization in esterification kettle |
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| CN202010509974.8A Pending CN111620779A (en) | 2020-06-08 | 2020-06-08 | Dibutyl phthalate production process capable of preventing crystallization in esterification kettle |
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Cited By (2)
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| CN114832758A (en) * | 2022-04-26 | 2022-08-02 | 浙江建业化工股份有限公司 | Production device and production method for de-activated carbon low-color diisobutyl phthalate |
| CN114933534A (en) * | 2022-04-28 | 2022-08-23 | 山东蓝帆化工有限公司 | Continuous esterification production process of diisooctyl terephthalate heterogeneous system |
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Application publication date: 20200904 |