CN107376805A - A kind of matrine petroleum ether crystal system and its production technology - Google Patents
A kind of matrine petroleum ether crystal system and its production technology Download PDFInfo
- Publication number
- CN107376805A CN107376805A CN201710691612.3A CN201710691612A CN107376805A CN 107376805 A CN107376805 A CN 107376805A CN 201710691612 A CN201710691612 A CN 201710691612A CN 107376805 A CN107376805 A CN 107376805A
- Authority
- CN
- China
- Prior art keywords
- reactor
- matrine
- crystallizing tank
- petroleum ether
- filter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
Abstract
The invention discloses a kind of matrine petroleum ether crystal system, including reactor, filter and crystallizing tank, the reactor, filter and crystallizing tank are set gradually, condenser is communicated with the top of the reactor, first solvent inlet, downtake pipe and the first manhole, centre at the top of the reactor is provided with the first motor, the second solvent inlet is communicated with the top of the crystallizing tank, second exhaust pipe and the second manhole, one end of the second shaft coupling is connected with the second bull stick, second bull stick is connected with the second agitating paddle through crystallizing tank and end, the outer wall of the crystallizing tank is covered with cooling water layer, water inlet pipe is connected with the left side wall of the cooling water layer, outlet pipe is connected with the right side wall of the cooling water layer, the bottom of the crystallizing tank is connected with the second discharge nozzle.Optimize crystallization processes, fade and crystallization is carried out simultaneously, ensure colour fading quality, save the time, carried out in the system of closing, it is safer.
Description
Technical field
The invention belongs to chemical technology field, more specifically, more particularly to a kind of matrine petroleum ether crystal system.Together
When, the invention further relates to a kind of matrine petroleum ether crystallization production process.
Background technology
The relation of the mankind and chemical industry is very close, spreads to the every aspect of life.In the modern life, almost at any time with
Ground all be unable to do without chemical products, from material lifes such as clothing, food, shelter, rows to culture and arts, the cultural life such as amusement, being required for
Chemical product services for it.Some chemical products play epoch-making important function in human development history.Their production and
Using, or even represent certain historical stage of human civilization.As domestic chemical industry is fast-developing, the production capacity of chemical products
Increase substantially.
Crystallization is the process that solute separates out from solution, can be divided into nucleus generation (nucleation) and two stages of crystal growth,
The motive force in two stages is all the degree of supersaturation (value of the concentration of solute more than its saturation solubility in crystallization solution) of solution.
The generation of nucleus has three kinds of forms:I.e. primary homogeneous nucleation, primary nonhomogen-ous nucleation and secondary nucleation.Under high degree of supersaturation,
Solution spontaneously generates the process of nucleus, referred to as primary homogeneous nucleation;Induction of the solution in exotic (micronic dust in such as air)
The process of lower generation nucleus, referred to as primary nonhomogen-ous nucleation;And the nucleation process in the solution containing solute crystals, referred to as two
Secondary nucleation.Secondary nucleation falls within nonhomogen-ous nucleation process, and it is between crystal or crystal and other solid (wall, stirrings
Device etc.) collision when caused tiny crystal grains induction under occur.
For the crystal system of matrine petroleum ether, traditional crystallization processes are complicated, fade not thorough, have very big office
It is sex-limited.
The content of the invention
The invention aims to solve shortcoming present in prior art, and a kind of matrine petroleum ether knot proposed
Crystallographic system is united and its production technology.
To achieve these goals, present invention employs following technical scheme:A kind of matrine petroleum ether crystal system, bag
Reactor, filter and crystallizing tank are included, the reactor, filter and crystallizing tank are set gradually, and are connected at the top of the reactor
It is connected with condenser, the first solvent inlet, downtake pipe and the first manhole, the centre at the top of the reactor is provided with the first electricity
Machine, the output end of first motor are connected with first shaft coupling, and one end of the first shaft coupling is connected with the first bull stick, institute
To state the first bull stick and be connected with the first agitating paddle through reactor and end, the bottom of the reactor is connected with the first discharge nozzle,
Connected between the reactor and filter by pipeline, the second solvent inlet, second row are communicated with the top of the crystallizing tank
Tracheae and the second manhole, the filter are connected to the second solvent inlet at the top of crystallizing tank by pipeline, the crystallizing tank
Top is provided with the second motor, and the output end of second motor is connected with second shaft coupling, one end of the second shaft coupling
The second bull stick is connected with, second bull stick is connected with the second agitating paddle, the outer wall of the crystallizing tank through crystallizing tank and end
Covered with cooling water layer, water inlet pipe is connected with the left side wall of the cooling water layer, is connected on the right side wall of the cooling water layer
There is outlet pipe, the bottom of the crystallizing tank is connected with the second discharge nozzle.
Preferably, the side wall of the reactor is provided with insulation construction layer, and the insulation construction layer is polyurethane structural layer,
The thickness of the insulation construction layer is not less than 10mm.
Preferably, first agitating paddle and the second agitating paddle are c-type, and first agitating paddle and the second agitating paddle are equal
Fixed by way of welding.
Preferably, the top of the reactor is also communicated with air gauge.
Preferably, the filter is stud filter.
Preferably, first solvent inlet, the first manhole, the second solvent inlet, the second manhole, the first discharge nozzle,
The end of two discharge nozzles, water inlet pipe and outlet pipe is welded with flange.
Present invention also offers a kind of matrine petroleum ether crystallization production process, comprise the following steps:
S1, petroleum ether is raised in reactor, be slowly stirred, added the thick alkali of matrine, begin heat to temperature in the kettle 50
DEG C, and activated carbon is added, persistently flow back 1h;
S2, by liquid in kettle by filter, activated carbon is filtered out, liquid is inserted in crystallizing tank;
S3, crystallizing tank are persistently slowly stirred, and to room temperature, stop stirring, stand 24h, and sediment fraction is matrine crystalline substance
Body.
A kind of matrine petroleum ether crystal system provided by the invention and its production technology, compared with prior art, make
Technique is simple, and petroleum ether is raised in reactor first, is slowly stirred, and adds the thick alkali of matrine, begins heat to temperature in the kettle
50 DEG C, and activated carbon is added, persistently flowed back 1h, and by filter liquid in kettle then is filtered out into activated carbon, then liquid is inserted
In crystallizing tank, crystallizing tank is persistently slowly stirred, and to room temperature, is stopped stirring, is stood 24h, sediment fraction is matrine crystal, is pressed
Aforesaid operations, with petroleum ether 200L, matrine thick alkali 20kg, activated carbon 10kg obtain graininess matrine crystalline solid 15.8kg, are in
White clear shape, through liquid chromatographic detection, matrine content 98.3%;It is thick with petroleum ether 400L, matrine by aforesaid operations
Alkali 40kg, activated carbon 20kg obtain graininess matrine crystalline solid 32.3kg, the white transparence of crystal, through liquid chromatographic detection,
Matrine content is 98.5%, optimizes crystallization processes, fades and crystallization is carried out simultaneously, ensure colour fading quality, save the time, sealing
Carried out in the system closed, it is safer, reduce enterprise's production cost.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention;
Fig. 2 and Fig. 3 is the chromatogram of matrine content of the present invention detection.
In figure:1 reactor, 2 filters, 3 crystallizing tanks, 4 condensers, 5 first solvent inlets, 6 downtake pipes, 7 first
Manhole, 8 air gauges, 9 first motors, 10 first shaft couplings, 11 first bull sticks, 12 first agitating paddles, 13 insulation construction layers, 14
One discharge nozzle, 15 second solvent inlets, 16 second exhaust pipes, 17 second manholes, 18 second motors, 19 second shaft couplings, 20
Two bull sticks, 21 second agitating paddles, 22 cooling water layers, 23 water inlet pipes, 24 outlet pipes, 25 second discharge nozzles.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.The specific embodiments described herein are merely illustrative of the present invention, is not used to limit
The present invention.
The invention provides a kind of matrine petroleum ether crystal system as shown in Figure 1, including reactor 1, the and of filter 2
Crystallizing tank 3, the reactor 1, filter 2 and crystallizing tank 3 are set gradually, the top of the reactor 1 be communicated with condenser 4,
First solvent inlet 5, the manhole 7 of downtake pipe 6 and first, the centre at the top of reactor 1 are provided with the first motor 9, institute
The output end for stating the first motor 9 is connected with first shaft coupling 10, and one end of the first shaft coupling 10 is connected with the first bull stick 11,
First bull stick 11 is connected with the first agitating paddle 12 through reactor 1 and end, and the bottom of the reactor 1 is connected with first
Discharge nozzle 14, connected between the reactor 1 and filter 2 by pipeline, the top of the crystallizing tank 3 is communicated with the second solvent
It is second molten to be connected to the top of crystallizing tank 3 by pipeline for import 15, the manhole 17 of second exhaust pipe 16 and second, the filter 2
Agent import 15, the top of the crystallizing tank 3 are provided with the second motor 18, and the output end of second motor 18 is connected with second
Axle device 19, one end of the second shaft coupling 19 are connected with the second bull stick 20, and second bull stick 20 runs through crystallizing tank 3 and end
It is connected with the second agitating paddle 21, the outer wall of the crystallizing tank 3 is covered with cooling water layer 22, on the left side wall of the cooling water layer 22
Water inlet pipe 23 is connected with, is connected with outlet pipe 24 on the right side wall of the cooling water layer 22, the bottom of the crystallizing tank 3 is connected with
Second discharge nozzle 25, the side wall of the reactor 1 are provided with insulation construction layer 13, and the insulation construction layer 13 is polyurethane structural
Layer, the thickness of the insulation construction layer 13 are not less than 10mm, and the agitating paddle 21 of the first agitating paddle 12 and second is c-type, institute
State the first agitating paddle 12 and the second agitating paddle 21 is fixed by way of welding, the top of the reactor 1 is also communicated with gas
Table 8 is pressed, the filter 2 is stud filter, first solvent inlet 5, the first manhole 7, the second solvent inlet 15, second
Manhole 17, the first discharge nozzle 14, the second discharge nozzle 25, the end of water inlet pipe 23 and outlet pipe 24 are welded with flange.
Present invention also offers a kind of matrine petroleum ether crystallization production process, comprise the following steps:
S1, petroleum ether is raised in reactor, be slowly stirred, added the thick alkali of matrine, begin heat to temperature in the kettle 50
DEG C, and activated carbon is added, persistently flow back 1h;
S2, by liquid in kettle by filter, activated carbon is filtered out, liquid is inserted in crystallizing tank;
S3, crystallizing tank are persistently slowly stirred, and to room temperature, stop stirring, stand 24h, and sediment fraction is matrine crystalline substance
Body.
In summary:Compared with prior art, petroleum ether is raised in reactor 1 first, be slowly stirred, add matrine
Thick alkali, 50 DEG C of temperature in the kettle is begun heat to, and add activated carbon, persistently flow back 1h, then by liquid in kettle by filter 2,
Activated carbon is filtered out, then liquid is inserted in crystallizing tank 3, crystallizing tank 3 is persistently slowly stirred, and to room temperature, is stopped stirring, is stood
24h, sediment fraction are matrine crystal, and by aforesaid operations, with petroleum ether 200L, matrine thick alkali 20kg, activated carbon 10kg are obtained
Graininess matrine crystalline solid 15.8kg, white transparence, through liquid chromatographic detection, matrine content 98.3%, chromatogram
Figure is as shown in Figure 2;By aforesaid operations, graininess matrine knot is obtained with petroleum ether 400L, matrine thick alkali 40kg, activated carbon 20kg
Crystal 32.3kg, the white transparence of crystal, through liquid chromatographic detection, matrine content 98.5%, chromatogram such as Fig. 3 institutes
Show;Optimize crystallization processes, fade and crystallization is carried out simultaneously, ensure colour fading quality, save the time, carried out in the system of closing,
It is safer.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of matrine petroleum ether crystal system, including reactor (1), filter (2) and crystallizing tank (3), it is characterised in that:
The reactor (1), filter (2) and crystallizing tank (3) are set gradually, and condenser is communicated with the top of the reactor (1)
(4), the first solvent inlet (5), downtake pipe (6) and the first manhole (7), the centre at the top of the reactor (1) are provided with
First motor (9), the output end of first motor (9) are connected with first shaft coupling (10), the first shaft coupling (10)
One end is connected with the first bull stick (11), and first bull stick (11) is connected with the first agitating paddle through reactor (1) and end
(12), the bottom of the reactor (1) is connected with the first discharge nozzle (14), passes through between the reactor (1) and filter (2)
Pipeline is connected, and the second solvent inlet (15), second exhaust pipe (16) and the second manhole are communicated with the top of the crystallizing tank (3)
(17), the filter (2) is connected to the second solvent inlet (15) at the top of crystallizing tank (3), the crystallizing tank (3) by pipeline
Top the second motor (18) is installed, the output end of second motor (18) is connected with second shaft coupling (19), described
One end of two shaft couplings (19) is connected with the second bull stick (20), and second bull stick (20) connects through crystallizing tank (3) and end
There is the second agitating paddle (21), the outer wall of the crystallizing tank (3) is covered with cooling water layer (22), the left side of the cooling water layer (22)
Water inlet pipe (23) is connected with wall, outlet pipe (24), the crystallizing tank (3) are connected with the right side wall of the cooling water layer (22)
Bottom be connected with the second discharge nozzle (25).
A kind of 2. matrine petroleum ether crystal system according to claim 1, it is characterised in that:The reactor (1)
Side wall is provided with insulation construction layer (13), and the insulation construction layer (13) is polyurethane structural layer, the insulation construction layer (13)
Thickness be not less than 10mm.
A kind of 3. matrine petroleum ether crystal system according to claim 1, it is characterised in that:First agitating paddle
(12) and the second agitating paddle (21) is c-type, and first agitating paddle (12) and the second agitating paddle (21) pass through the side of welding
Formula is fixed.
A kind of 4. matrine petroleum ether crystal system according to claim 1, it is characterised in that:The reactor (1)
Top is also communicated with air gauge (8).
A kind of 5. matrine petroleum ether crystal system according to claim 1, it is characterised in that:The filter (2) is
Stud filter.
A kind of 6. matrine petroleum ether crystal system according to claim 1, it is characterised in that:First solvent inlet
(5), the first manhole (7), the second solvent inlet (15), the second manhole (17), the first discharge nozzle (14), the second discharge nozzle (25),
The end of water inlet pipe (23) and outlet pipe (24) is welded with flange.
7. the matrine petroleum ether crystallization production process described in a kind of claim 1, it is characterised in that comprise the following steps:
S1, petroleum ether is raised in reactor, be slowly stirred, added the thick alkali of matrine, begin heat to 50 DEG C of temperature in the kettle, and
Activated carbon is added, persistently flow back 1h;
S2, by liquid in kettle by filter, activated carbon is filtered out, liquid is inserted in crystallizing tank;
S3, crystallizing tank are persistently slowly stirred, and to room temperature, are stopped stirring, are stood 24h, sediment fraction is matrine crystal.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109569459A (en) * | 2018-11-09 | 2019-04-05 | 昆明理工大学 | A kind of warehouse separated type reacting furnace suitable for salting out method |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102391136A (en) * | 2011-10-27 | 2012-03-28 | 东营市冠森绝缘制品有限公司 | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process |
CN102617575A (en) * | 2012-04-10 | 2012-08-01 | 宁夏紫荆花制药有限公司 | Preparation process of high-purity oxymatrine |
CN102633798A (en) * | 2012-04-26 | 2012-08-15 | 宁夏紫荆花制药有限公司 | Method for preparing high-purity matrine from sophora alopecuroides |
CN102786523A (en) * | 2012-07-19 | 2012-11-21 | 宁夏紫荆花制药有限公司 | Technology for preparing sophocarpine from Sophora alopecuroides L |
CN104130285A (en) * | 2014-08-01 | 2014-11-05 | 浙江阿尔法化工科技有限公司 | Continuous production process of 3-hydroxyphenyl phosphoroso-propanoic acid and production system thereof |
-
2017
- 2017-08-14 CN CN201710691612.3A patent/CN107376805A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102391136A (en) * | 2011-10-27 | 2012-03-28 | 东营市冠森绝缘制品有限公司 | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process |
CN102617575A (en) * | 2012-04-10 | 2012-08-01 | 宁夏紫荆花制药有限公司 | Preparation process of high-purity oxymatrine |
CN102633798A (en) * | 2012-04-26 | 2012-08-15 | 宁夏紫荆花制药有限公司 | Method for preparing high-purity matrine from sophora alopecuroides |
CN102786523A (en) * | 2012-07-19 | 2012-11-21 | 宁夏紫荆花制药有限公司 | Technology for preparing sophocarpine from Sophora alopecuroides L |
CN104130285A (en) * | 2014-08-01 | 2014-11-05 | 浙江阿尔法化工科技有限公司 | Continuous production process of 3-hydroxyphenyl phosphoroso-propanoic acid and production system thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109569459A (en) * | 2018-11-09 | 2019-04-05 | 昆明理工大学 | A kind of warehouse separated type reacting furnace suitable for salting out method |
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Application publication date: 20171124 |