CN104447340B - DOP esterification system and production technique - Google Patents
DOP esterification system and production technique Download PDFInfo
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- CN104447340B CN104447340B CN201410547238.6A CN201410547238A CN104447340B CN 104447340 B CN104447340 B CN 104447340B CN 201410547238 A CN201410547238 A CN 201410547238A CN 104447340 B CN104447340 B CN 104447340B
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- 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
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- 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
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Abstract
The present invention relates to DOP esterification system and production technique.It comprises reactor, reactor two ends are provided with input channel, reactor is communicated with riser, riser is communicated with esterification column, esterification column upper end is connected with the first cooling emendation, first cooling emendation side is connected with alcohol-water separation tank by the first holding tank, is connected with lime set pump between the first holding tank and alcohol-water separation tank.DOP esterification production technology comprises 1) esterification step; 2) alcohol operation is rushed; 3) neutralization &washing operation; 4) dehydration procedure; 5) filter progress.The invention has the advantages that: cooling emendation can improve the efficiency of cooling, reduce the working hour of a whole set of operation, achieve the recycle of water resources in whole technological process simultaneously, save softening water consumption in production cost, decrease sewage discharge simultaneously.In addition, by the dewatering process condition after adjustment neutralization &washing, effectively can reduce generation water and return into the impact of neutralization &washing on product, guarantee the top grade rate of DOP product.
Description
Technical field
The invention belongs to DOP production technical field, relate to a kind of DOP esterification system and production technique.
Background technology
DOP softening agent belongs to the one in additives for plastics, be a kind of can with the chemical of plastics or synthetic resins compatibility, it can make plastics deliquescing and reduce fragility, thus industrially has a wide range of applications.Because dioctyl phthalate (DOP) (be called for short DOP) has excellent performance and cheap, and raw material is easy to get, thus its industrially the most conventional system technique synthesis DOP comprise acid catalysis synthesis and non-acid catalyzes and synthesizes; Phthalic anhydride and octanol have a certain amount of generation water and produce in the process of esterification output DOP, and general enterprise is all fallen generating water (generate in water and carry a small amount of octanol) as discharge of wastewater, affects to environmental improvement.
In order to reduce the discharge of waste water, the people propose various technical scheme, and such as Chinese patent literature discloses a kind of DOP continuous production technology [patent No.: 201110208523.1; Notification number: 102295564A] it comprises the steps: that phthalic anhydride, isooctyl alcohol and titanate catalyst are first through esterification, then through dealcoholysis, neutralization &washing, stripping drying, adsorption filtration, obtains DOP.The identical esterifying kettle of structure that this technical scheme is connected by employing 6 carries out esterification, and keep alcohol excessive, transformation efficiency is high, is greater than 99.5%, thick ester acid number≤0.3mgKOH/g that reaction generates, alcohol excess 16%; By using the program, obtain less energy-consumption, high production capacity and the production method of continuous esterification, transformation efficiency is high, improves the production output of device, decreases production cost, be suitable for suitability for industrialized production; Alcohol excess, the water that Esterification Stage generates, recycle, synthetical recovery, decreases the generation of " three wastes ".Although this technical scheme improves reactivity, there is no accomplish better effect for technology such as alcohol-water separation, have the top grade rate of certain DOP product, but process is comparatively complicated, production cost is high.
Summary of the invention
The object of the invention is for the problems referred to above, provide one can improve esterification reaction rate, reduce the reaction times, decrease the DOP esterification system of sewage discharge.
For achieving the above object, present invention employs following technical proposal: DOP esterification system, comprise the reactor that can store mixed solution, reactor two ends are provided with input channel, and this mixed solution comprises phthalic anhydride, octanol and catalyzer, it is characterized in that, reactor is communicated with riser, and riser is communicated with esterification column, and esterification column upper end is connected with the first cooling emendation, first cooling emendation side is connected with alcohol-water separation tank by the first holding tank, is connected with lime set pump between the first holding tank and alcohol-water separation tank.
In above-mentioned DOP esterification system, the upper end of described alcohol-water separation tank is connected with reclaims alcohol pipe, and the lower end of alcohol-water separation tank is connected with waste water tank; The opposite side of waste water tank is directly communicated with the pipeline of input liquid caustic soda, and this pipeline is connected to reactor.
In above-mentioned DOP esterification system, described input channel outside surface is provided with reactor well heater.
In above-mentioned DOP esterification system, the first described cooling emendation comprises the first process water cooler and the second process water cooler of two series connection, and the second process water cooler side is connected with the second holding tank.
In above-mentioned DOP esterification system, be communicated with the first holding tank bottom the second described holding tank.
In above-mentioned DOP esterification system, the upper and lower two ends of described reactor are connected with thick ester pump by some pipelines, and thick ester pump is also connected with the second cooling emendation.
In above-mentioned DOP esterification system, the second described cooling emendation is two water coolers in parallel.
Another object of the present invention is for the problems referred to above, provides a kind of and simplifies, for producing the high DOP of top grade rate technique with low cost.
For reaching another object above-mentioned, present invention employs following technical proposal: a kind of DOP esterification production technology, is characterized in that, comprise the following steps:
1) esterification step; Check cleaning esterifying kettle facility, confirm that whether all pipelines of the esterifying kettle that will feed in raw material, valve be intact, whether opening and closing is correct, after confirming the unlatching situation of valve, start feedstock pump, the start-stop of control pump is carried out by esterifying kettle under meter, DD oil in head tank is thrown in relevant esterifying kettle, closes material inlet valve, in esterifying kettle, carry out esterification respectively by pump housing input phthalic anhydride and octanol.
2) alcohol operation is rushed; Phthalic anhydride and octanol are in middle esterification, and generation water, alcohol rise to condensation, then squeezes in alcohol-water separation tank by lime set pump in esterification column, and alcohol water is separated in alcohol-water separation tank.
3) neutralization &washing operation; Generation water waste water pump in waste water tank is squeezed in esterifying kettle, participates in neutralization &washing and use.
4) dehydration procedure;
5) filter progress.
In above-mentioned DOP esterification production technology, in the process inputting phthalic anhydride and octanol, be heated to 60 °-75 ° by reactor well heater.
In above-mentioned DOP esterification production technology, the moisture component content in described DD oil is below 0.9%.
Compared with prior art, the invention has the advantages that: this apparatus structure is tight, cooling emendation can improve the efficiency of cooling, reduce the working hour of a whole set of operation, during work, esterification is generated water and return neutralization &washing operation as washing softening water use, both reclaimed and generated a small amount of octanol carried in water, and achieved the recycle of water resources in whole technological process simultaneously, save softening water consumption in production cost, decrease sewage discharge simultaneously.In addition, by the dewatering process condition after adjustment neutralization &washing, effectively can reduce generation water and return into the impact of neutralization &washing on product, guarantee the top grade rate of DOP product.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the schematic diagram of invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one
As shown in Figure 1, DOP esterification system, comprise the reactor 1 that can store mixed solution, reactor two ends are provided with input channel 2, and this mixed solution comprises phthalic anhydride, octanol and catalyzer; Reactor is communicated with riser 3, riser is communicated with esterification column 4, esterification column upper end is connected with the first cooling emendation 5, the first described cooling emendation comprises the first process water cooler 6 and the second process water cooler 7 of two series connection, and be all communicated with the first holding tank 8, second process water cooler side is connected with the second holding tank 9, is communicated with bottom the second described holding tank with the first holding tank.First cooling emendation side is connected with alcohol-water separation tank 10 by the first holding tank, is connected with lime set pump 11 between the first holding tank and alcohol-water separation tank; The upper end of alcohol-water separation tank is connected with reclaims alcohol pipe, and the lower end of alcohol-water separation tank is connected with waste water tank 12; The opposite side of waste water tank is directly communicated with the pipeline 13 of input liquid caustic soda, and this pipeline is connected to reactor.By the connection of waste water tank and reactor, the waste water produced in production process can be recycled, in addition, this waste water tank is also connected with supplementary water supply pipe, if it is not enough to produce waste water, supplement by tap water.
The upper and lower two ends of described reactor are connected with thick ester pump 14 by some pipelines, and thick ester pump is also connected with the second cooling emendation 15; The second described cooling emendation is two water coolers in parallel.The thick ester directly produced in a kettle. is first extracted by thick ester pump 16, cooling, can continue to keep the inner reaction fully of reactor by vacating space timely.
Another object of the present invention is for the problems referred to above, provides a kind of and simplifies, for producing the high DOP of top grade rate technique with low cost.
For reaching another object above-mentioned, present invention employs following technical proposal: a kind of DOP esterification production technology, is characterized in that, comprise the following steps:
1) esterification step; Check cleaning esterifying kettle facility, confirm that whether all pipelines of the esterifying kettle that will feed in raw material, valve be intact, whether opening and closing is correct, after confirming the unlatching situation of valve, start feedstock pump, carried out the start-stop of control pump by esterifying kettle under meter, the DD oil in head tank is thrown in relevant esterifying kettle, close material inlet valve, moisture component content in requirement DD oil, below 0.9%, carries out esterification respectively by pump housing input phthalic anhydride and octanol in esterifying kettle; In the process inputting phthalic anhydride and octanol, be heated to 60 ° by reactor well heater.
2) alcohol operation is rushed; Phthalic anhydride and octanol are in middle esterification, and generation water, alcohol rise to condensation, then squeezes in alcohol-water separation tank by lime set pump in esterification column, and alcohol water is separated in alcohol-water separation tank.
3) neutralization &washing operation; Generation water waste water pump in waste water tank is squeezed in esterifying kettle, participates in neutralization &washing and use.
4) dehydration procedure;
5) filter progress.
Embodiment two
As shown in Figure 1, DOP esterification system, comprise the reactor 1 that can store mixed solution, reactor two ends are provided with input channel 2, and this mixed solution comprises phthalic anhydride, octanol and catalyzer; Reactor is communicated with riser 3, riser is communicated with esterification column 4, esterification column upper end is connected with the first cooling emendation 5, the first described cooling emendation comprises the first process water cooler 6 and the second process water cooler 7 of two series connection, and be all communicated with the first holding tank 8, second process water cooler side is connected with the second holding tank 9, is communicated with bottom the second described holding tank with the first holding tank.First cooling emendation side is connected with alcohol-water separation tank 10 by the first holding tank, is connected with lime set pump 11 between the first holding tank and alcohol-water separation tank; The upper end of alcohol-water separation tank is connected with reclaims alcohol pipe, and the lower end of alcohol-water separation tank is connected with waste water tank 12; The opposite side of waste water tank is directly communicated with the pipeline 13 of input liquid caustic soda, and this pipeline is connected to reactor.By the connection of waste water tank and reactor, the waste water produced in production process can be recycled, in addition, this waste water tank is also connected with supplementary water supply pipe, if it is not enough to produce waste water, supplement by tap water.
The upper and lower two ends of described reactor are connected with thick ester pump 14 by some pipelines, and thick ester pump is also connected with the second cooling emendation 15; The second described cooling emendation is two water coolers in parallel.The thick ester directly produced in a kettle. is first extracted by thick ester pump 16, cooling, can continue to keep the inner reaction fully of reactor by vacating space timely.
Another object of the present invention is for the problems referred to above, provides a kind of and simplifies, for producing the high DOP of top grade rate technique with low cost.
For reaching another object above-mentioned, present invention employs following technical proposal: a kind of DOP esterification production technology, is characterized in that, comprise the following steps:
1) esterification step; Check cleaning esterifying kettle facility, confirm that whether all pipelines of the esterifying kettle that will feed in raw material, valve be intact, whether opening and closing is correct, after confirming the unlatching situation of valve, start feedstock pump, carried out the start-stop of control pump by esterifying kettle under meter, the DD oil in head tank is thrown in relevant esterifying kettle, close material inlet valve, moisture component content in requirement DD oil, below 0.5%, carries out esterification respectively by pump housing input phthalic anhydride and octanol in esterifying kettle; In the process inputting phthalic anhydride and octanol, be heated to 75 ° by reactor well heater.
2) alcohol operation is rushed; Phthalic anhydride and octanol are in middle esterification, and generation water, alcohol rise to condensation, then squeezes in alcohol-water separation tank by lime set pump in esterification column, and alcohol water is separated in alcohol-water separation tank.
3) neutralization &washing operation; Generation water waste water pump in waste water tank is squeezed in esterifying kettle, participates in neutralization &washing and use.
4) dehydration procedure;
5) filter progress.
Embodiment three
As shown in Figure 1, DOP esterification system, comprise the reactor 1 that can store mixed solution, reactor two ends are provided with input channel 2, and this mixed solution comprises phthalic anhydride, octanol and catalyzer; Reactor is communicated with riser 3, riser is communicated with esterification column 4, esterification column upper end is connected with the first cooling emendation 5, the first described cooling emendation comprises the first process water cooler 6 and the second process water cooler 7 of two series connection, and be all communicated with the first holding tank 8, second process water cooler side is connected with the second holding tank 9, is communicated with bottom the second described holding tank with the first holding tank.First cooling emendation side is connected with alcohol-water separation tank 10 by the first holding tank, is connected with lime set pump 11 between the first holding tank and alcohol-water separation tank; The upper end of alcohol-water separation tank is connected with reclaims alcohol pipe, and the lower end of alcohol-water separation tank is connected with waste water tank 12; The opposite side of waste water tank is directly communicated with the pipeline 13 of input liquid caustic soda, and this pipeline is connected to reactor.By the connection of waste water tank and reactor, the waste water produced in production process can be recycled, in addition, this waste water tank is also connected with supplementary water supply pipe, if it is not enough to produce waste water, supplement by tap water.
The upper and lower two ends of described reactor are connected with thick ester pump 14 by some pipelines, and thick ester pump is also connected with the second cooling emendation 15; The second described cooling emendation is two water coolers in parallel.The thick ester directly produced in a kettle. is first extracted by thick ester pump 16, cooling, can continue to keep the inner reaction fully of reactor by vacating space timely.
Another object of the present invention is for the problems referred to above, provides a kind of and simplifies, for producing the high DOP of top grade rate technique with low cost.
For reaching another object above-mentioned, present invention employs following technical proposal: a kind of DOP esterification production technology, is characterized in that, comprise the following steps:
1) esterification step; Check cleaning esterifying kettle facility, confirm that whether all pipelines of the esterifying kettle that will feed in raw material, valve be intact, whether opening and closing is correct, after confirming the unlatching situation of valve, start feedstock pump, carried out the start-stop of control pump by esterifying kettle under meter, the DD oil in head tank is thrown in relevant esterifying kettle, close material inlet valve, moisture component content in requirement DD oil, 0.4%, carries out esterification respectively by pump housing input phthalic anhydride and octanol in esterifying kettle; In the process inputting phthalic anhydride and octanol, be heated to 73 ° by reactor well heater.
2) alcohol operation is rushed; Phthalic anhydride and octanol are in middle esterification, and generation water, alcohol rise to condensation, then squeezes in alcohol-water separation tank by lime set pump in esterification column, and alcohol water is separated in alcohol-water separation tank.
3) neutralization &washing operation; Generation water waste water pump in waste water tank is squeezed in esterifying kettle, participates in neutralization &washing and use.
4) dehydration procedure;
5) filter progress.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1.DOP esterification system, comprise the reactor that can store mixed solution, reactor two ends are provided with input channel, this mixed solution comprises phthalic anhydride, octanol and catalyzer, and reactor is communicated with riser, and riser is communicated with esterification column, it is characterized in that, esterification column upper end is connected with the first cooling emendation, and the first cooling emendation side is connected with alcohol-water separation tank by the first holding tank, is connected with lime set pump between the first holding tank and alcohol-water separation tank; Wherein, the upper end of alcohol-water separation tank is connected with reclaims alcohol pipe, and the lower end of alcohol-water separation tank is connected with waste water tank; The opposite side of waste water tank is directly communicated with the pipeline of input liquid caustic soda, and this pipeline is connected to reactor; The upper and lower two ends of reactor are connected with thick ester pump by some pipelines, and thick ester pump is also connected with the second cooling emendation.
2. according to the DOP esterification system described in claim 1, it is characterized in that, described input channel outside surface is provided with reactor well heater.
3. according to the DOP esterification system described in claim 1, it is characterized in that, the first described cooling emendation comprises the first process water cooler and the second process water cooler of two series connection, and the second process water cooler side is connected with the second holding tank.
4. according to the DOP esterification system described in claim 3, it is characterized in that, be communicated with the first holding tank bottom the second described holding tank.
5. according to the DOP esterification system described in claim 1, it is characterized in that, the second described cooling emendation is two water coolers in parallel.
6. the DOP esterification production technology utilizing the DOP esterification system of claim 1 to 5 described in any one to carry out, is characterized in that, comprise the following steps:
1) esterification step; Check cleaning esterifying kettle facility, confirm that whether all pipelines of the esterifying kettle that will feed in raw material, valve be intact, whether opening and closing is correct, after confirming the unlatching situation of valve, start feedstock pump, the start-stop of control pump is carried out by esterifying kettle under meter, DD oil in head tank is thrown in relevant esterifying kettle, closes material inlet valve, in esterifying kettle, carry out esterification respectively by pump housing input phthalic anhydride and octanol;
2) alcohol operation is rushed; The esterification in esterifying kettle of phthalic anhydride and octanol, generation water, alcohol rise to condensation, then squeeze in alcohol-water separation tank by lime set pump in esterification column, and alcohol water is separated in alcohol-water separation tank;
3) neutralization &washing operation; Generation water waste water pump in waste water tank is squeezed in esterifying kettle, participates in neutralization &washing and use;
4) dehydration procedure;
5) filter progress.
7., according to the DOP esterification production technology described in claim 6, it is characterized in that, described step 2) rush in alcohol operation, in the process inputting phthalic anhydride and octanol, be heated to 60 °-75 ° by reactor well heater.
8., according to the DOP esterification production technology described in claim 6, it is characterized in that, described step 1) in esterification step, the moisture component content in described DD oil is below 0.9%.
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| CN105566105A (en) * | 2016-02-16 | 2016-05-11 | 濮阳市盛源能源科技股份有限公司 | Production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester |
| CN111620779A (en) * | 2020-06-08 | 2020-09-04 | 福建春达化工有限公司 | Dibutyl phthalate production process capable of preventing crystallization in esterification kettle |
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| CN204589034U (en) * | 2014-10-16 | 2015-08-26 | 杭州宇田科技有限公司 | A kind of DOP esterification system |
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Effective date of registration: 20190305 Address after: 310000 Linjiang High-tech Industrial Park, Hangzhou City, Zhejiang Province, No. 1788 Jingsi Road Patentee after: Hangzhou Fleming Technology Co., Ltd. Address before: 311228 No. 1788 Jingsi Road, Xiaoshan Linjiang Industrial Park, Hangzhou City, Zhejiang Province Patentee before: HANGZHOU YUTIAN TECHNOLOGY CO., LTD. |
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Address after: 310000 no.1788, Jingsi Road, Linjiang high tech Industrial Park, Hangzhou, Zhejiang Province Patentee after: Hangzhou Fulai anthracite Technology Co., Ltd Address before: 310000 Linjiang High-tech Industrial Park, Hangzhou City, Zhejiang Province, No. 1788 Jingsi Road Patentee before: Hangzhou Fleming Technology Co., Ltd. |
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