CN105111077B - A kind of method for reclaiming solvent in trimethylolpropane light component - Google Patents
A kind of method for reclaiming solvent in trimethylolpropane light component Download PDFInfo
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- CN105111077B CN105111077B CN201510436527.3A CN201510436527A CN105111077B CN 105111077 B CN105111077 B CN 105111077B CN 201510436527 A CN201510436527 A CN 201510436527A CN 105111077 B CN105111077 B CN 105111077B
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- solvent
- butyl acetate
- light component
- filter
- trimethylolpropane
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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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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method for reclaiming solvent in trimethylolpropane light component, it is characterised in that the step is：N-butyl acetate is added into crystallization kettle with trimethylolpropane light component first, crystallization kettle is kept in 55 DEG C of 1 2h of thermostatical crystallization；Material in crystallization kettle is delivered in filter and is filtered, obtain filtrate and filter cake, filtrate is transported to de- ester tower removing n-butyl acetate, n-butyl acetate is evaporated from after the condensation of condensed device group to be recovered to n-butyl acetate storage tank and recycles, and de- ester bottom of towe obtains high-purity solvent and returns solvent tank recycling.Different from impurity crystalline temperature using solvent, the light component containing a large amount of solvents is passed through in crystallization kettle with ester and is crystallized, then carries out filtering for crystallizing by filter, obtains the solvent containing ester and filter cake（Crystalline solid）, the solvent of high-load can be obtained after Crystallization Separation, finally solvent and ester is separated by de- ester tower again, so as to realize the maximization of the rate of recovery of solvent.
Description
Technical field
The present invention relates to a kind of method for reclaiming solvent in trimethylolpropane light component, belongs to technical field of fine
In purification part.
Background technology
Will be using a kind of esters solvent the trimethylolpropane in concentrate and double in trimethylolpropane production process
The organic matters such as trimethylolpropane are extracted, then solvent purifications are clean through solvent rectifying and de- light industry sequence, so as to
To the trimethylolpropane product of high-load, wherein the purpose of de- light industry sequence is to slough the acetal and half that solvent and side reaction are produced
The light components such as acetal, due to containing more solvent in light component, if selling directly as waste material, product cost can be improved
A lot, domestic at present is usually that the solvent in light component is purified recycling again using solvent recycling operation.
The method can reclaim a certain amount of solvent, but in place of Shortcomings：
1. recovered solvent purity it is difficult to ensure that, because impurity is more or less the same with the boiling point of solvent in light component, so as to lead
The solvent of extraction is caused also to contain a small amount of impurity, the length meeting of time one solvent slop storage tank causes extraction process effect to be deteriorated.
2. the solvent of bottom of towe and impurity azeotropic cause separating-purifying not thorough, and final bottom of towe is by the solvent containing 10%-15%
It is thrown away.
3. the energy is wasted, because the boiling point of solvent is higher, is needed under negative pressure to be raised to 180 DEG C and just be can guarantee that bottom of towe solvent contains
, below 15%, separation costs are slightly higher for amount.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method for reclaiming solvent in trimethylolpropane light component, profit
The solvent of high-load very big the characteristics of from light component is as far as possible recovered to while again not with impurity crystalline temperature difference with solvent
Need too big cost.
To solve above-mentioned technical problem, the technical scheme is that：It is molten in a kind of recovery trimethylolpropane light component
The method of agent, its innovative point are that the step is：Step S1：80 DEG C -100 DEG C of n-butyl acetate is added into crystallization kettle first
It is interior；And add and n-butyl acetate trimethylolpropane light component identical in quality in crystallization kettle, trimethylolpropane light component
In contain the solvent for utilizing to be recycled；Step S2：After having added trimethylolpropane light component, crystallization kettle is kept in 55 DEG C of constant temperature
Crystallization 1-2h；Step S3：Material in crystallization kettle is delivered in filter and is filtered, when beginning is filtered first by filter
One Matter Transfer loop of composition is connected by circulating line with crystallization kettle, material is passed through into Matter Transfer circuit cycle then
1h-1.5h, is then filtered, and is filtered and is continued 0.5h-1h, obtains filtrate and filter cake, filtrate is delivered to filtrate tanks；Step
Rapid S4：The filter cake being filtrated to get in step S3 is warming up to 60 DEG C -80 DEG C to be melted in filter, while entering filter
Row is evacuated to -0.095 MPa～-0.098MPa, duration 0.5h～1h, will be the n-butyl acetate removing in filter cake dry
Only, obtain the light component without solvent and n-butyl acetate；Step S5：Filtrate is transported to de- ester tower removing n-butyl acetate, second
Sour N-butyl is evaporated from after the condensation of condensed device group to be recovered to n-butyl acetate storage tank and recycles, and de- ester bottom of towe obtains high-purity
Solvent returns solvent tank recycling.
Preferably, in step S3, after the completion of filtration, filter 15min-30min is purged using nitrogen.
It is an advantage of the current invention that：
（1）In the present invention, different from impurity crystalline temperature using solvent, the light component containing a large amount of solvents is passed through knot with ester
Crystallized in brilliant kettle, then filtering for crystallizing is carried out by filter, obtained the solvent containing ester and filter cake（Crystalline solid）, by knot
The solvent of high-load can be obtained after brilliant separation, finally solvent and ester is separated by de- ester tower again；Sent out by detection, chemical examination
Now take off the solvent ＞ more than 99% of ester bottom of towe, and the solvent ＜ 1% in filter cake, so as to realize solvent the rate of recovery most
Bigization.
（2）Energy saving, traditional solvent recycling will be warmed up to 180 DEG C or so, as long as now taking off ester tower is raised to 80-120
99% solvent is can be obtained by between DEG C, energy consumption declines to a great extent.And the chilled water needed for crystallizing is common with trimethylolpropane section
With, therefore expense is reduced than individually upper ice maker.
（3）The expense of equipment needed thereby is decreased obviously, and traditional solvent recycling wants to reach separation purpose, and recycling tower will
Ask very high, highly in more than 25m, cost is high, and the de- ester tower of the present invention is due to technological requirement, which needs 10m or so, more traditional
Cost of equipment reduce many.
（4）In the present invention, by carrying out being warming up to 80 DEG C or so to filter cake, solvent-laden light component is melted,
Vacuumized simultaneously, can be clean by the ester removing in filter cake, the light component without solvent and ester is obtained, returning for light component is realized
Receive and recycle.Resource utilization is substantially increased, it is more environmentally-friendly.
Specific embodiment
Embodiment one
Step S1：N-butyl acetate first by 3t temperature at 80 DEG C is added in crystallization kettle；And add in the crystallization kettle with
N-butyl acetate trimethylolpropane light component identical in quality, in trimethylolpropane light component containing it is to be recycled utilize it is molten
Agent, in light component, solvent is 70% or so；
Step S2：After having added trimethylolpropane light component, crystallization kettle is kept in 55 DEG C of thermostatical crystallization 1h；
Step S3：Material in crystallization kettle is delivered in filter and is filtered, when beginning is filtered first by filter
One Matter Transfer loop of composition is connected by circulating line with crystallization kettle, material is passed through into Matter Transfer circuit cycle then
1h, is then filtered, and is filtered and is continued 1h, obtains filtrate and filter cake, filtrate is delivered to filtrate tanks, is used after the completion of filtration
Nitrogen purges filter 15min；In this step, filtrate contains most of n-butyl acetate of solvent to be recycled and addition,
And main component is the light component containing a small amount of n-butyl acetate in filter cake；
Step S4：The filter cake being filtrated to get in step S3 is warming up to 80 DEG C to be melted in filter, while to mistake
Filter carries out being evacuated to -0.098MPa, duration 1h, will be the n-butyl acetate removing in filter cake clean, obtains without molten
Agent and the light component of n-butyl acetate；
Step S5：Filtrate is transported to de- ester tower removing n-butyl acetate, and n-butyl acetate is evaporated cold from condensed device group
N-butyl acetate storage tank is recovered to after solidifying to recycle, de- ester bottom of towe obtains high-purity solvent and returns solvent tank recycling.
The solvent that de- ester bottom of towe is obtained is detected as content 99.3%, and yield is 2.1T, and it is sharp that solvent returns solvent tank repetition
With, the n-butyl acetate for steaming, after condenser cooling, the refluxing portion kettle that decrystallizes in part is recycled.
Embodiment two
Step S1：N-butyl acetate first by 3T temperature at 80 DEG C is added in crystallization kettle；And add in the crystallization kettle with
3T trimethylolpropane light components, contain the solvent for utilizing to be recycled in trimethylolpropane light component, contain solvent in light component
60%。
Step S2：After having added trimethylolpropane light component, crystallization kettle is kept in 55 DEG C of thermostatical crystallization 1h；
Step S3：Material in crystallization kettle is delivered in filter and is filtered, when beginning is filtered first by filter
One Matter Transfer loop of composition is connected by circulating line with crystallization kettle, material is passed through into Matter Transfer circuit cycle then
1h, is then filtered, and is filtered and is continued 1h, obtains filtrate and filter cake, filtrate is delivered to filtrate tanks, is used after the completion of filtration
Nitrogen purges filter 15min；In this step, filtrate contains most of n-butyl acetate of solvent to be recycled and addition,
And main component is the light component containing a small amount of n-butyl acetate in filter cake；
Step S4：The filter cake being filtrated to get in step S3 is warming up to 80 DEG C to be melted in filter, while to mistake
Filter carries out being evacuated to -0.098MPa, duration 1h, will be the n-butyl acetate removing in filter cake clean, obtains without molten
Agent and the light component of n-butyl acetate；
Step S5：Filtrate is transported to de- ester tower removing n-butyl acetate, and n-butyl acetate is evaporated cold from condensed device group
N-butyl acetate storage tank is recovered to after solidifying to recycle, de- ester bottom of towe obtains high-purity solvent and returns solvent tank recycling.
The solvent that de- ester bottom of towe is obtained is detected as content 99.1%, and yield is 1.8T, and it is sharp that solvent returns solvent tank repetition
With, the n-butyl acetate for steaming, after condenser cooling, the refluxing portion kettle that decrystallizes in part is recycled.
Embodiment three
Step S1：N-butyl acetate first by 5T temperature at 80 DEG C is added in crystallization kettle；And add in the crystallization kettle with
5T trimethylolpropane light components, contain the solvent for utilizing to be recycled in trimethylolpropane light component；In light component, solvent contains
Measure as 70% or so.
Step S2：After having added trimethylolpropane light component, crystallization kettle is kept in 55 DEG C of thermostatical crystallization 1h；
Step S3：Material in crystallization kettle is delivered in filter and is filtered, when beginning is filtered first by filter
One Matter Transfer loop of composition is connected by circulating line with crystallization kettle, material is passed through into Matter Transfer circuit cycle then
1h, is then filtered, and is filtered and is continued 1h, obtains filtrate and filter cake, filtrate is delivered to filtrate tanks, is used after the completion of filtration
Nitrogen purges filter 15min；In this step, filtrate contains most of n-butyl acetate of solvent to be recycled and addition,
And main component is the light component containing a small amount of n-butyl acetate in filter cake；
Step S4：The filter cake being filtrated to get in step S3 is warming up to 80 DEG C to be melted in filter, while to mistake
Filter carries out being evacuated to -0.098MPa, duration 1h, will be the n-butyl acetate removing in filter cake clean, obtains without molten
Agent and the light component of n-butyl acetate；
Step S5：Filtrate is transported to de- ester tower removing n-butyl acetate, and n-butyl acetate is evaporated cold from condensed device group
N-butyl acetate storage tank is recovered to after solidifying to recycle, de- ester bottom of towe obtains high-purity solvent and returns solvent tank recycling.
The solvent that de- ester bottom of towe is obtained is detected as content 99.0%, and yield is 3.5T, and it is sharp that solvent returns solvent tank repetition
With, the n-butyl acetate for steaming, after condenser cooling, the refluxing portion kettle that decrystallizes in part is recycled.
Claims (2)
1. a kind of method for reclaiming solvent in trimethylolpropane light component, it is characterised in that the step is：
Step S1：First 80 DEG C -100 DEG C of n-butyl acetate is added in crystallization kettle；And just add with acetic acid in crystallization kettle
Butyl ester trimethylolpropane light component identical in quality, contains the solvent for utilizing to be recycled in trimethylolpropane light component；
Step S2：After having added trimethylolpropane light component, crystallization kettle is kept in 55 DEG C of thermostatical crystallization 1-2h；
Step S3：Material in crystallization kettle is delivered in filter and is filtered, when beginning is filtered first by filter and knot
Brilliant kettle constitutes a Matter Transfer loop by circulating line connection, and material is passed through Matter Transfer circuit cycle 1h- then
1.5h, is then filtered, and is filtered and is continued 0.5h-1h, obtains filtrate and filter cake, filtrate is delivered to filtrate tanks；
Step S4：The filter cake being filtrated to get in step S3 is warming up to 60 DEG C -80 DEG C to be melted in filter, while to mistake
Filter carries out being evacuated to -0.095 MPa～-0.098MPa, duration 0.5h～1h, by the n-butyl acetate in filter cake
Removing is clean, obtains the light component without solvent and n-butyl acetate；
Step S5：Filtrate is transported to de- ester tower removing n-butyl acetate, and n-butyl acetate is evaporated, from after the condensation of condenser group,
It is recovered to n-butyl acetate storage tank to recycle, the solvent that de- ester bottom of towe is obtained returns solvent tank recycling.
2. it is according to claim 1 reclaim trimethylolpropane light component in solvent method, it is characterised in that：The step
In rapid S3, after the completion of filtration, filter 15min-30min is purged using nitrogen.
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| CN201510436527.3A CN105111077B (en) | 2015-07-23 | 2015-07-23 | A kind of method for reclaiming solvent in trimethylolpropane light component |
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| CN105111077A CN105111077A (en) | 2015-12-02 |
| CN105111077B true CN105111077B (en) | 2017-03-29 |
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| KR101852214B1 (en) * | 2010-09-07 | 2018-04-25 | 미츠비시 가스 가가쿠 가부시키가이샤 | Method for producing ditrimethylolpropane |
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Address after: 226200 Changjiang Town, Rugao City, Rugao, Nantong, Jiangsu, No. 6, Xiangjiang Road Co-patentee after: Jiangsu hundred Sichuan high science and technology new materials Limited by Share Ltd Patentee after: Nantong hundred Sichuan new materials Co., Ltd. Co-patentee after: Rugao ran chemical materials Co., Ltd. Address before: 226500 Rugao, Jiangsu City, the Yangtze River town (Rugao port) Shannon Road, No. 6 Co-patentee before: Wuxi Baichuan Chemical Industrial Co., Ltd. Patentee before: Baichuan Chemical (Rugao) Co., Ltd. Co-patentee before: Hundred river chemical industry are sold Rugao company limited |