CN103130645A - Device and method for preparing 1, 2-cyclohexane diamyl phthalate - Google Patents
Device and method for preparing 1, 2-cyclohexane diamyl phthalate Download PDFInfo
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- CN103130645A CN103130645A CN2013100156227A CN201310015622A CN103130645A CN 103130645 A CN103130645 A CN 103130645A CN 2013100156227 A CN2013100156227 A CN 2013100156227A CN 201310015622 A CN201310015622 A CN 201310015622A CN 103130645 A CN103130645 A CN 103130645A
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Abstract
The invention discloses a device for preparing 1, 2- cyclohexane diamyl phthalate. The device comprises an esterification kettle, a refining kettle, a filtering tank and a hydrogenation reaction unit. The hydrogenation reaction unit comprises an intermediate tank, a hydrogen compressing device and a hydrogenation reactor and further comprises a gas-liquid separation system. The intermediate tank is provided with a solution heater, the hydrogenation reactor is connected with the intermediate tank, and the gas-liquid separation system is connected with the hydrogenation reaction unit. The invention further discloses a preparation method. The preparation method includes the steps of esterification, neutralization, washing, refining and hydrogenation reacting. Compared with the prior art, the device for preparing the 1, 2-cyclohexane diamyl phthalate has the advantages of being applied to industrial large-scale production, low in cost and high in efficiency. The 1, 2-cyclohexane diamyl phthalate has a good toxicological property, is well compatible with polyvinyl chloride (PVC), odorless, environment-friendly and non-toxic. In the process of pelleting or plastifying, the 1, 2-cyclohexane diamyl phthalate is compatible with PVC materials quite well, low in viscosity and capable of being applied to a specific injection mold so that the service cycle of a plastification product is prolonged, and a final product is very low in mobility after plastified by the 1, 2-clohexane diamyl phthalate.
Description
Technical field
The present invention relates to a kind ofly prepare 1, the devices and methods therefor of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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 wherein take the phthalate fluidizer as main body, has accounted for 75% share more than 8,000,000 tons.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 concentrates on the pregnancy period rat and is 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 present invention is directed to deficiency of the prior art, provide a kind of preparation 1 that is applicable to industrial mass production, the device of 2-cyclohexane cyclohexanedimethanodibasic diamyl ester.
for solving the problems of the technologies described above, the present invention is solved by following technical proposals: a kind ofly prepare 1, the device of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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, be provided with paddle on this stir shaft, the outer end of described paddle is rotatably connected to movable plate, have torsion spring between described paddle and described movable plate, and an end of described movable plate contacts with the inwall of described esterifying kettle.Device of the present invention is applicable to industrial mass production, have advantages of that production cost is low, and movable plate contacts the inwall of esterifying kettle all the time under the effect of torsion spring, can remove the inwall of clean esterifying kettle, and torsion spring damages movable plate and esterifying kettle inwall can avoid having the outstanding material that is difficult to strike off on the esterifying kettle inwall time.
As preferably, the height of above-mentioned movable plate is greater than the height of described paddle.The area that this programme can make movable plate remove is larger, and elimination efficiency is higher.
the present invention also provides a kind of preparation 1 that is applicable to industrial mass production simultaneously, the method of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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 amylalcohol, after putting into catalyzer, input is faced phthalate anhydride, wherein, face phthalate anhydride and amylalcohol charging capacity mol ratio is 1:3, feed intake complete, close solid dog-house and nitrogen, begin 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 the heating of described refining kettle vacuum and 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 measures 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, deliver to the battery limit (BL) finally by after cooling 40 ℃ of reactor product cooler, namely obtain finished product 1,2-cyclohexane cyclohexanedimethanodibasic diamyl 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, removes the 4.5MPa separating tank through the isolated liquid phase of described circulation gas 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 invention has the beneficial effects as follows: 1) product of the present invention 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 invention 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, product of the present invention is fairly good with PVC material compatibleness; 4) product viscosity of the present invention 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 invention 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 invention 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 present invention is described in further detail: embodiment 1: a kind ofly prepare 1, the device of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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, has torsion spring 24 between described paddle 18 and described 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.Evenly offer some holes 23 on the blade face of this paddle 18, these some holes 23 comprise the circular port that evenly is arranged at edge, described stirring blade face.Mixing effect is good, and the blade face is stressed even everywhere.
Wherein, the angle on the medullary ray in above-mentioned hole 23 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 diamyl 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 amylalcohol, after putting into catalyzer, input is faced phthalate anhydride, wherein, face phthalate anhydride and amylalcohol charging capacity mol ratio is 1:3, feed intake complete, close solid dog-house and nitrogen, begin 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 the heating of described refining kettle vacuum and 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 measures 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, removes the 4.5MPa separating tank through the isolated liquid phase of described circulation gas 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, deliver to the battery limit (BL) finally by after cooling 40 ℃ of reactor product cooler, namely obtain finished product 1,2-cyclohexane cyclohexanedimethanodibasic diamyl ester.
Claims (4)
1. one kind prepares 1, the device of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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, has torsion spring between described paddle and described 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 diamyl ester according to claim 1, it is characterized in that: the height of described movable plate is greater than the height of described paddle.
3. one kind is used device as claimed in claim 1 to prepare 1, the method of 2-cyclohexane cyclohexanedimethanodibasic diamyl 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 amylalcohol, after putting into catalyzer, input is faced phthalate anhydride, wherein, face phthalate anhydride and amylalcohol charging capacity mol ratio is 1:3, feed intake complete, close solid dog-house and nitrogen, begin 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 the heating of described refining kettle vacuum and 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 measures 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, deliver to the battery limit (BL) finally by after cooling 40 ℃ of reactor product cooler, namely obtain finished product 1,2-cyclohexane cyclohexanedimethanodibasic diamyl ester.
4. a kind of device according to claim 3 prepares 1, the method of 2-cyclohexane cyclohexanedimethanodibasic diamyl ester, it is characterized in that: described 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, remove the 4.5MPa separating tank through the isolated liquid phase of described circulation gas 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.
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| CN201310015622.7A CN103130645B (en) | 2013-01-16 | 2013-01-16 | Device and method for preparing 1, 2-cyclohexane diamyl phthalate |
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| CN201310015622.7A CN103130645B (en) | 2013-01-16 | 2013-01-16 | Device and method for preparing 1, 2-cyclohexane diamyl phthalate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223631A (en) * | 1996-06-28 | 1999-07-21 | 新日本理化株式会社 | Process for the preparation of cyclohexanedimethanol |
| CN101417950A (en) * | 2008-10-27 | 2009-04-29 | 中国科学院大连化学物理研究所 | Method for preparing 1,2-cyclohexane cyclohexanedimethanol dibasic ester |
| CN203284356U (en) * | 2013-01-16 | 2013-11-13 | 宁波东来化工有限公司 | Device for preparing 1, 2-disubstituted cyclohexane two formic acid two amyl |
-
2013
- 2013-01-16 CN CN201310015622.7A patent/CN103130645B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1223631A (en) * | 1996-06-28 | 1999-07-21 | 新日本理化株式会社 | Process for the preparation of cyclohexanedimethanol |
| CN101417950A (en) * | 2008-10-27 | 2009-04-29 | 中国科学院大连化学物理研究所 | Method for preparing 1,2-cyclohexane cyclohexanedimethanol dibasic ester |
| CN203284356U (en) * | 2013-01-16 | 2013-11-13 | 宁波东来化工有限公司 | Device for preparing 1, 2-disubstituted cyclohexane two formic acid two amyl |
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