CN203284355U - Device for preparing 1, 2-disubstituted cyclohexane phthalate group - Google Patents
Device for preparing 1, 2-disubstituted cyclohexane phthalate group Download PDFInfo
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- CN203284355U CN203284355U CN2013200222084U CN201320022208U CN203284355U CN 203284355 U CN203284355 U CN 203284355U CN 2013200222084 U CN2013200222084 U CN 2013200222084U CN 201320022208 U CN201320022208 U CN 201320022208U CN 203284355 U CN203284355 U CN 203284355U
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Abstract
The utility model discloses a device for preparing a 1, 2-disubstituted cyclohexane phthalate group, which comprises a esterification kettle, a refining kettle, a filtering pot and a hydrogenation unit, wherein the hydrogenation unit comprises a middle pot with a solution heater, hydrogen compression equipment, the hydrogenation reactor connected with the middle pot and a gas liquid separation system connected with the hydrogenation unit. Compared with the prior art, the device provided by the utility model is suitable for mass production, low in cost and high in efficiency, has a better toxicology characteristic, and better consistency to PVC, is odor-free, environment-friendly, and non-poisonous; during the process of prilling or plastification production, the device has better compatibility with PVC materials; the device is low in viscosity, and suitable for specific injection mould, so that service life of a plastification product is prolonged; the finished product of the plastification product of the device is low in mobility.
Description
Technical field
The utility model relates to and a kind ofly prepares 1, the device of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, this product is applicable to the responsive flexible PVC products such as pad, Sport ﹠ Casual product, sealing agent, shower curtain, footwear, slipmat, water pipe, electric wire toy, food product pack, medical treatment product in food fresh keeping membrane, food sealing, can be used for producing toy for children below three years old, also can be used for low peculiar smell automobile and contact gloves, the indoor wallpaper of environment-friendly type, decorative sheets of material, intravenously blood transfusion tube and Medical blood bag etc. with cable, medical nutrition supply pipe, adhesive membrane, domestic food.
Background technology
In life, softening agent is ubiquitous, except plastic bottle, tableware, daily necessities, toy, even also can contain softening agent in preservative film.Fluidizer is widely used in the Industrial products such as food product pack, medical and hygiene article, paint, also has the phthalate things such as denier DEHP in environment, tap water.Softening agent is consumption maximum in all additives for plasticss.Wherein the use of the phthalate of cost performance optimum is the most extensive, and global annual usage quantity, more than 8,000,000 tons,, wherein take the phthalate fluidizer as main body, has accounted for 75% share.It can increase the suppleness of plastics.But adjacent benzene class softening agent easily escapes in environment, and what at this moment bring into play is all the bad effect of environment incretion interferent.Fluidizer can enter human body by approach such as Digestive tract, respiratory system and skin contact, has genotoxicity and development toxicity, and this harm is also hidden and very long.The focus that recently scientific research is paid close attention to, mainly concentrate on the pregnancy period rat and be exposed in the phthalate material,, by the intergenerational impact that placenta and lactication produce, is mainly the impact that the Development of Reproductive System on its male offspring produces.Although the human toxicity data are abundant not enough at present, that keeps someone at a respectful distance, throws and abandon worldwide reaches common understanding.Adjacent benzene class fluidizer consumption is huge, use range is wide, contaminated area and the number that affects are just all luxuriant is considerable, and phthalate can be described as a distribution on global class synthetic environment pollutent the most widely at present, can detect in air, water, soil and dust.Phthalate has inrichment at the organism escheat, and the significantly residue of this compounds is arranged in aquatic organism, and final people expose wherein by approach such as food and air.
Summary of the invention
The utility model, for deficiency of the prior art, provides a kind of preparation 1 that is applicable to industrial mass production, the device of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester.
for solving the problems of the technologies described above, the utility model is solved by following technical proposals: a kind ofly prepare 1, the device of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, comprise esterifying kettle, refining kettle, hay tank and hydrogenation reaction unit, described hydrogenation reaction unit comprises the tundish that are provided with solution heater, the hydrogen gas booster compressor, the hydrogenator that is connected with described tundish, an outlet of described hydrogen gas booster compressor is communicated with the lower section catalyst bed of described hydrogenator, another outlet communication loop hydrogen preheater, described circulating hydrogen preheater communication loop hydrogen well heater, described circulating hydrogen well heater is communicated with described hydrogenator, described hydrogenator is connected with hp flash drum, one of them outlet of described hp flash drum connects the 4.5MPa separating tank, another outlet ligation device water cooler, described reactor water cooler connects the circulation gas separating tank, one of them outlet of described circulation gas separating tank connects described hydrogen gas booster compressor, another outlet connects boiler systems, also have an outlet to connect described 4.5MPa separating tank, one of them outlet of described 4.5MPa separating tank connects described boiler plant, another outlet is connected with low pressure flash chamber, one of them outlet of described low pressure flash chamber connects described boiler systems, another outlet connects the decolouring groove, described decolouring groove is connected with reactor product cooler, be provided with stir shaft in wherein said esterifying kettle, be provided with paddle on this stir shaft, the outer end of described paddle is rotatably connected to movable plate, and the height of this movable plate is greater than the height of described paddle, and an end of described movable plate contacts with the inwall of described esterifying kettle.Device of the present utility model is applicable to industrial mass production, have advantages of that production cost is low, and the movable plate on paddle is rotatably connected on paddle, when stir shaft rotates, the inwall of movable plate contact esterifying kettle under the effect of centrifugal force, can be clean with removing on the esterifying kettle inwall, prevent its encrustation.
the utility model also provides a kind of preparation 1 that is applicable to industrial mass production simultaneously, the method of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, it is characterized in that comprising the following steps: 1) esterification: open nitrogen and pass into described esterifying kettle, after air drains, open and stir, drop into decyl alcohol, after putting into catalyzer, input is faced phthalate anhydride, wherein, face phthalate anhydride and decyl alcohol charging capacity mol ratio is 1:3, feed intake complete, close solid dog-house and nitrogen, start to heat up, carry out esterification, be warming up to 220 ℃ ~ 230 ℃, when the esterification acid number reaches 1mgKOH/g when following, esterification finishes, steam off, open cooling water temperature to 100 ℃, change described refining kettle over to vacuum, 2) neutralization, washing: open described refining kettle and stir, pump into the buck for preparing in described refining kettle, neutralize, material is with after liquid caustic soda fully mixes, stop stirring, standing minute water, acid number reaches below 0.05mgKOH/g, open and stir, pump into esterification generation water and a small amount of steam condensation water in described refining kettle, wash stir about 10min, stop stirring standing minute water, 3) refining: minute water is complete, opens described refining kettle vacuum and the heating of described refining kettle, more than treating that vacuum tightness reaches negative 0.09Mpa, be warming up to 170 ~ 175 ℃, pass into open steam in described refining kettle, carry out stripping, stripping 240min, close open steam, flash-point is surveyed in sampling, after flash-point is qualified, open nitrogen at the bottom of described refining kettle, dry 30min, measure moisture content of finished products content and acid number, pumps into described hay tank after qualified to filter, 4) hydrogenation: material after filtering enters described tundish, be forced into 12.9MPa through the raw material fresh feed pump, being steam heated to 200 ℃ through described solution heater by 3.0MPa again advances hydrogenator and carries out hydrogenation reaction, from the circulating hydrogen after the de-oiling of hydrogen gas booster compressor, a part rises to 180 ℃ in circulating hydrogen preheater temperature, be steam heated to 200 ℃ through the circulating hydrogen well heater by 3.0MPa again and advance hydrogenator and carry out hydrogenation reaction, a part is removed hydrogenator lower section catalyst bed as cold hydrogen, reflect material mixture through gas-liquid separation, after liquidus temperature is down to 100 ℃, enters the decolouring groove and decolour and take off heavily, finally by after cooling 40 ℃ of reactor product cooler, deliver to battery limit (BL), namely obtain finished product 1,2-cyclohexane cyclohexanedimethanodibasic didecyl ester.
As preferably, above-mentioned gas-liquid separation comprises the following steps: reflect material mixture after hp flash drum carries out gas-liquid separation, gas phase temperature after interchanger and circulating hydrogen heat exchange is down to 84 ℃ by 215 ℃, again through the reaction gas water cooler by circulating water to 40 ℃, then go the circulation gas separating tank to carry out gas-liquid separation, through the isolated gas phase major part of described circulation gas separating tank as recycle hydrogen dehydrogenation air pressure contracting equipment, the part gas phase is removed boiler systems, through the isolated liquid phase of described circulation gas separating tank, removes the 4.5MPa separating tank after being decompressed to 4.5MPa; From the hp flash drum liquid phase after being decompressed to 4.5MPa with the interchanger heat exchange after temperature be down to 80 ℃ by 215 ℃, go described 4.5MPa separating tank to carry out gas-liquid separation, the flashed vapour gas that goes to act as a fuel removes boiler systems, and liquid phase goes low pressure flash chamber to carry out gas-liquid separation through being decompressed to 0.4MPa; The flashed vapour of the low pressure flash chamber gas that acts as a fuel after being decompressed to 0.3MPa removes boiler systems, after liquidus temperature is down to 100 ℃, enters the decolouring groove and decolours and take off heavily.
Compared with prior art, the beneficial effects of the utility model are: 1) product of the present utility model is through rigorous toxicity test, and the toxicological characteristics of its excellence makes it to be applicable to the responsive flexible PVC products such as toy, food product pack, medical treatment product; 2) product of the present utility model has fine consistency to PVC, has the low-temperature performance of good processing characteristics, low volatility, excellence, and odorlessness, environment-protecting asepsis; 3) when granulation or plasticising production, the utility model product is fairly good with PVC material compatibleness; 4) the utility model product viscosity is low,, applicable to specific injection mould, even can be used for very accurate careful design, thereby extends the life cycle of plastified prod; 5) the finished product transport property of product plasticising of the present utility model is very low, can with the safe combinations of resin material such as ABS, SAN, PC, guarantee that product has long work-ing life and excellent properties; 6) apparatus and method of the present utility model are suitable for large-scale industrialization production, and production cost is low, and production efficiency is high.
Description of drawings
Fig. 1 is workflow schematic diagram of the present invention.
Fig. 2 is the structural representation of esterifying kettle in the present invention.
Embodiment
below in conjunction with embodiment, the utility model is described in further detail: embodiment 1: a kind ofly prepare 1, the device of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, comprise esterifying kettle 1, refining kettle 2, hay tank 3 and hydrogenation reaction unit, described hydrogenation reaction unit comprises the tundish 4 that are provided with solution heater, hydrogen gas booster compressor 6, the hydrogenator 5 that is connected with described tundish 4, an outlet of described hydrogen gas booster compressor 6 is communicated with the lower section catalyst bed of described hydrogenator 5, another outlet communication loop hydrogen preheater 7, described circulating hydrogen preheater 7 communication loop hydrogen well heaters 8, described circulating hydrogen well heater 8 is communicated with described hydrogenator 5, described hydrogenator 5 is connected with hp flash drum 9, one of them outlet of described hp flash drum 9 connects 4.5MPa separating tank 13, another outlet ligation device water cooler 10, described reactor water cooler 10 connects circulation gas separating tank 11, described circulation gas separating tank 11 one of them outlet connect described hydrogen gas booster compressor 6, another outlet connects boiler systems 12, also have an outlet to connect described 4.5MPa separating tank 13, one of them outlet of described 4.5MPa separating tank 13 connects described boiler systems 12, another outlet is connected with low pressure flash chamber 14, one of them outlet of described low pressure flash chamber 14 connects described boiler systems 12, another outlet connects decolouring groove 15, described decolouring groove 15 is connected with reactor product cooler 16, be provided with stir shaft 17 in wherein said esterifying kettle 1, be provided with paddle 18 on this stir shaft 17, the outer end of described paddle 18 is rotatably connected to movable plate 22, the height of this movable plate 22 is greater than the height of described paddle 18, and an end of described movable plate 22 contacts with the inwall of described esterifying kettle 1.
Also evenly offer some holes on the blade face of this paddle 18, these some holes comprise that one is arranged at the RC circular port 19 in described paddle blade face, and some aplysia punctatas that are are distributed in the kidney slot 20 around described circular port 19 and are arranged on aperture 21 between two adjacent described kidney slots 20.Mixing effect is good, and the paddle blade face is stressed even everywhere.
Wherein, the angle on the medullary ray in above-mentioned hole and described paddle 18 blade faces is less than 90 degree.
embodiment 2, a kind of preparation 1 that is applicable to industrial mass production, the method of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, it is characterized in that comprising the following steps: 1) esterification: open nitrogen and pass into described esterifying kettle, after air drains, open and stir, drop into decyl alcohol, after putting into catalyzer, input is faced phthalate anhydride, wherein, face phthalate anhydride and decyl alcohol charging capacity mol ratio is 1:3, feed intake complete, close solid dog-house and nitrogen, start to heat up, carry out esterification, be warming up to 220 ℃ ~ 230 ℃, when the esterification acid number reaches 1mgKOH/g when following, esterification finishes, steam off, open cooling water temperature to 100 ℃, change described refining kettle over to vacuum, 2) neutralization, washing: open described refining kettle and stir, pump into the buck for preparing in described refining kettle, neutralize, material is with after liquid caustic soda fully mixes, stop stirring, standing minute water, acid number reaches below 0.05mgKOH/g, open and stir, pump into esterification generation water and a small amount of steam condensation water in described refining kettle, wash stir about 10min, stop stirring standing minute water, 3) refining: minute water is complete, opens described refining kettle vacuum and the heating of described refining kettle, more than treating that vacuum tightness reaches negative 0.09Mpa, be warming up to 170 ~ 175 ℃, pass into open steam in described refining kettle, carry out stripping, stripping 240min, close open steam, flash-point is surveyed in sampling, after flash-point is qualified, open nitrogen at the bottom of described refining kettle, dry 30min, measure moisture content of finished products content and acid number, pumps into described hay tank after qualified to filter, 4) hydrogenation: material after filtering enters described tundish, be forced into 12.9MPa through the raw material fresh feed pump, being steam heated to 200 ℃ through described solution heater by 3.0MPa again advances hydrogenator and carries out hydrogenation reaction, from the circulating hydrogen after the de-oiling of hydrogen gas booster compressor, a part rises to 180 ℃ in circulating hydrogen preheater temperature, be steam heated to 200 ℃ through the circulating hydrogen well heater by 3.0MPa again and advance hydrogenator and carry out hydrogenation reaction, a part is removed hydrogenator lower section catalyst bed as cold hydrogen, reflect material mixture after hp flash drum carries out gas-liquid separation, gas phase temperature after interchanger and circulating hydrogen heat exchange is down to 84 ℃ by 215 ℃, again through the reaction gas water cooler by circulating water to 40 ℃, then go the circulation gas separating tank to carry out gas-liquid separation, through the isolated gas phase major part of described circulation gas separating tank as recycle hydrogen dehydrogenation air pressure contracting equipment, the part gas phase is removed boiler systems, through the isolated liquid phase of described circulation gas separating tank, removes the 4.5MPa separating tank after being decompressed to 4.5MPa, from the hp flash drum liquid phase after being decompressed to 4.5MPa with the interchanger heat exchange after temperature be down to 80 ℃ by 215 ℃, go described 4.5MPa separating tank to carry out gas-liquid separation, the flashed vapour gas that goes to act as a fuel removes boiler systems, and liquid phase goes low pressure flash chamber to carry out gas-liquid separation through being decompressed to 0.4MPa, the flashed vapour of the low pressure flash chamber gas that acts as a fuel after being decompressed to 0.3MPa removes boiler systems, after liquidus temperature is down to 100 ℃, enters the decolouring groove and decolour and take off heavily, finally by after cooling 40 ℃ of reactor product cooler, deliver to battery limit (BL), namely obtain finished product 1,2-cyclohexane cyclohexanedimethanodibasic didecyl ester.
Claims (2)
1. one kind prepares 1, the device of 2-cyclohexane cyclohexanedimethanodibasic didecyl ester, it is characterized in that: comprise esterifying kettle, refining kettle, hay tank and hydrogenation reaction unit, described hydrogenation reaction unit comprises the tundish that are provided with solution heater, the hydrogen gas booster compressor, the hydrogenator that is connected with described tundish, an outlet of described hydrogen gas booster compressor is communicated with the lower section catalyst bed of described hydrogenator, another outlet communication loop hydrogen preheater, described circulating hydrogen preheater communication loop hydrogen well heater, described circulating hydrogen well heater is communicated with described hydrogenator, described hydrogenator is connected with hp flash drum, one of them outlet of described hp flash drum connects the 4.5MPa separating tank, another outlet ligation device water cooler, described reactor water cooler connects the circulation gas separating tank, one of them outlet of described circulation gas separating tank connects described hydrogen gas booster compressor, another outlet connects boiler systems, also have an outlet to connect described 4.5MPa separating tank, one of them outlet of described 4.5MPa separating tank connects described boiler plant, another outlet is connected with low pressure flash chamber, one of them outlet of described low pressure flash chamber connects described boiler systems, another outlet connects the decolouring groove, described decolouring groove is connected with reactor product cooler, be provided with stir shaft in wherein said esterifying kettle, be provided with paddle on this stir shaft, the outer end of described paddle is rotatably connected to movable plate, and an end of described movable plate contacts with the inwall of described esterifying kettle.
2. a kind of device for preparing 1,2-cyclohexane cyclohexanedimethanodibasic didecyl ester according to claim 1, it is characterized in that: the height of described movable plate is greater than the height of described paddle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013200222084U CN203284355U (en) | 2013-01-16 | 2013-01-16 | Device for preparing 1, 2-disubstituted cyclohexane phthalate group |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013200222084U CN203284355U (en) | 2013-01-16 | 2013-01-16 | Device for preparing 1, 2-disubstituted cyclohexane phthalate group |
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| CN203284355U true CN203284355U (en) | 2013-11-13 |
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| CN2013200222084U Withdrawn - After Issue CN203284355U (en) | 2013-01-16 | 2013-01-16 | Device for preparing 1, 2-disubstituted cyclohexane phthalate group |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130640A (en) * | 2013-01-16 | 2013-06-05 | 宁波东来化工有限公司 | Device and method for preparing 1, 2-cyclohexane didecyl phthalate |
-
2013
- 2013-01-16 CN CN2013200222084U patent/CN203284355U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130640A (en) * | 2013-01-16 | 2013-06-05 | 宁波东来化工有限公司 | Device and method for preparing 1, 2-cyclohexane didecyl phthalate |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20131113 Effective date of abandoning: 20150610 |
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| RGAV | Abandon patent right to avoid regrant |