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 PDF

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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
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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.)
Pending
Application number
CN201710691612.3A
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Chinese (zh)
Inventor
侯引军
张开庆
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Shaanxi Xu Ang Biological Technology Co Ltd
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Shaanxi Xu Ang Biological Technology Co Ltd
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Publication date
Application filed by Shaanxi Xu Ang Biological Technology Co Ltd filed Critical Shaanxi Xu Ang Biological Technology Co Ltd
Priority to CN201710691612.3A priority Critical patent/CN107376805A/en
Publication of CN107376805A publication Critical patent/CN107376805A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0013Crystallisation cooling by heat exchange by indirect heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0059General arrangements of crystallisation plant, e.g. flow sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D471/00Heterocyclic 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
    • C07D471/22Heterocyclic 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

A kind of matrine petroleum ether crystal system and its production technology
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.
CN201710691612.3A 2017-08-14 2017-08-14 A kind of matrine petroleum ether crystal system and its production technology Pending CN107376805A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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