CN102380336A - Reactor for producing material easy to produce powder, and preparation method of the material - Google Patents
Reactor for producing material easy to produce powder, and preparation method of the material Download PDFInfo
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- CN102380336A CN102380336A CN2011102634313A CN201110263431A CN102380336A CN 102380336 A CN102380336 A CN 102380336A CN 2011102634313 A CN2011102634313 A CN 2011102634313A CN 201110263431 A CN201110263431 A CN 201110263431A CN 102380336 A CN102380336 A CN 102380336A
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Abstract
The invention discloses a reactor for producing a material easy to produce powder, and a preparation method of the material. One end of a rotary drum (1) is provided with a feed inlet (2). The other end of the rotary drum (1) is provided with a manhole (3). An outer side of the rotary drum (1) is connected to a rotating ring. An inner escape pipe is connected to a static ring. The reactor for producing a material easy to produce powder is characterized in that one end of a vacuum-pumping pipe (5) stretches into the rotary drum (1); the other end of the vacuum-pumping pipe (5) is connected to a vacuum pump (10); and a nitrogen inlet pipe (4) stretches into the rotary drum (1) and is utilized for conveying nitrogen into the rotary drum (1). The preparation method comprises the following steps that a dust-containing oligomer is added into the rotary drum (1) and is subjected to solid phase tackifying; high-purity nitrogen is fed into the rotary drum (1) and undergoes a reaction until the dust-containing oligomer no longer releases a mass of micromolecules; a vacuum-pumping process is carried out until pressure is below 80Pa; and the materials in the rotary drum (1) undergo a reaction until desired viscosity is obtained. The preparation method has the advantages that in the early stage, usually, material tackifying is realized through nitrogen addition, and thus pipe blocking caused by deposition of a mass of low-molecular weight and small-size powder particles produced in the rotary drum (1) is avoided; and in the later stage, complete oligomer solid phase tackifying is realized through vacuum-pumping, and thus a product yield is improved and a cost is reduced.
Description
Technical field
The present invention relates to a kind of agitated reactor, particularly a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder; The invention still further relates to a kind of method that is prepared in the material that has been prone to powder in the course of reaction.
Background technology
When producing special engineering plastics; The at present normal method that adopts be to prepare oligomer earlier, and again with the oligomer solid-phase tack producing, but high-temperature nylon and liquid crystal etc. can produce a large amount of undersized powders in that oligomer is processed when suitable dimension carries out solid-phase tack producing; Because rotary drum adopts and vacuumizes tackify usually; Thereby the low molecule that these undersized powders join regular meeting and the generation often of solid-phase tack producing in the rotary drum extracted out by high vacuum together, and the undersized powder that contains assorted oligomer can be deposited in the pipeline of vacuum-pumping tube, causes pipeline obstruction; Further tackify can cause the material its colour changed into yellow simultaneously.
Chinese patent 200810024815.8 discloses a kind of small solid-phase tack producing device and method for using thereof; Its method is polyester slice to be passed through in the charge door access arrangement, and make section begin polycondensation reaction after being heated to uniform temperature; And discharge with low-molecular material; The lower-molecular substance that course of reaction produced is discharged from charge door or vaccum exhaust outlet with nitrogen, and its advantage is that it is low that product is stablized energy consumption; But its deficiency is, only is fit to produced in small quantities and can not be applied to large-scale industrial circle.
Introduced the preparation method of nylon 6 slice in one piece " nylon solid-phase tack producing technology " (modern plastics processed and applied) by name; Comprise tackifying resin added in the rotary drum vacuumizing, carrying out tackify behind the nitrogen replacement again that its weak point is that tackify efficient is low and utilize not exclusively.
The scheme that solves at present generally is to be employed in the rotary drum before the tackify Powder screen to be fallen; But oligomer and still wall friction do not reach to collide each other and still can produce certain dust before viscosity gets on; The rotary drum solid-phase tack producing there is certain influence; And the undersized powder that sieves can cause waste, improves product cost.
Summary of the invention
The objective of the invention is to, a kind of agitated reactor is provided, can reduce dust and micromolecular quantity in the agitated reactor greatly,, another object of the present invention is to provide the method that has been prone to the material of powder in a kind of preparation feedback process to avoid line clogging.
A kind of agitated reactor of producing the material that in course of reaction, has been prone to powder has charge door on the rotary drum, the outer side joint rotating ring of rotary drum; Inner escape pipe connects stationary ring; One vacuum-pumping tube stretches into the rotary drum top, and its other end connects vavuum pump, and the nitrogen air inlet pipe stretches into the bottom of the drum can be to rotary drum delivered inside nitrogen.
In addition, a vacuum flap is arranged on the mouth of pipe of vacuum-pumping tube; The input of nitrogen air inlet pipe is equipped with a valve; One cyclone separator and a cold-trap are housed between vacuum-pumping tube and the vavuum pump; In the rotary drum, the mouth of pipe of nitrogen air inlet pipe is positioned at the bottom of the drum, and the vacuum-pumping tube mouth of pipe is positioned at the rotary drum top.
Be prone to the method for the material of powder in a kind of course of reaction, the oligomer that will contain dust joins and carries out solid-phase tack producing in the rotary drum, and earlier logical high pure nitrogen is reacted to oligomer and discharges little molecule no longer in a large number, is evacuated to reaction to said viscosity below the 80pa again.
Wherein, The particle diameter of oligomer greater than the material of 50um more than 90%; There is a large amount of hanging down to adopt logical nitrogen tackify when molecules produce early stage in the solid-phase tack producing reaction; Temperature, the time of logical nitrogen decide by the smoke amount of nitrogen outlet, the low molecule that produces in the solid-phase tack producing reaction later stage seldom the time employing vacuumize tackify.
There is a large amount of hanging down to adopt logical nitrogen tackify when molecules produce early stage in the solid-phase tack producing reaction; Temperature, the time of logical nitrogen are decided by the smoke amount of nitrogen outlet; The nitrogen throughput can not taken a large amount of dust out of with normal temperature and be advisable from the gas outlet, the low molecule that produces in the solid-phase tack producing reaction later stage adopts seldom the time again and vacuumizes tackify.Described tackify reaction both can be carried out at normal temperatures, also can under the heating of heating, carry out temperature required selection as required.
The method and the agitated reactor of the material of powder have been prone in the preparation feedback process according to the invention; Its advantage is: early stage, the modes of logical nitrogen that rely on made the material tackify more, blocked pipeline in the pipeline to avoid in the rotary drum a large amount of low molecules that produce and undersized powder to be deposited on; Later stage makes that through the mode that vacuumizes the oligomer solid-phase tack producing is complete, reduces cost when can improve the yield of product like this.
Description of drawings
Fig. 1 is a kind of solid-phase tack producing agitated reactor of producing the material that in course of reaction, has been prone to powder.
The specific embodiment
Through the specific embodiment the present invention is described below, but is not limited to this.
A kind of agitated reactor of producing the material that in course of reaction, has been prone to powder; On its rotary drum 1 charge door 2 is arranged; Rotary drum 1 outer side joint rotating ring, inner turnover tracheae connects stationary ring, and a vacuum-pumping tube 5 stretches in the rotary drum 1; Its other end connects vavuum pump 10, and nitrogen air inlet pipe 4 stretches into can be to rotary drum 1 delivered inside nitrogen in the rotary drum 1; One vacuum flap 6 is arranged on the mouth of pipe of vacuum-pumping tube 5; The input of nitrogen air inlet pipe 4 is equipped with a valve 7, and cyclone separator 8 and cold-trap 9 are housed between vacuum-pumping tube 5 and the vavuum pump 10; In the rotary drum, the mouth of pipe of nitrogen air inlet pipe is positioned at the bottom of the drum, and the vacuum-pumping tube mouth of pipe is positioned at the rotary drum top.
Its concrete production method is following:
The high-temperature nylon oligomer 10kg that will contain dust joins and carries out solid-phase tack producing in the 50L rotary drum, and wherein particle diameter is greater than the material 9kg of 50um, and particle diameter is less than the material 1kg of 50um; Get into the logical nitrogen of pipe from nitrogen, rotate rotary drum, be warming up to 210 ℃ after; Smoke is not obvious, switches to vacuum, is evacuated to 30Pa; At 260 ℃ of reactions 6 hours, cooling discharge.Discharging 9.8kg records relative viscosity 2.3 altogether.
The liquid crystal oligomer 10kg that will contain dust joins and carries out solid-phase tack producing in the 50L rotary drum, and wherein particle diameter is greater than the material 9kg of 50um, and particle diameter is less than the material 1kg of 50um; From the logical nitrogen of nitrogen air inlet pipe, rotate rotary drum, be warming up to 260 ℃; Smoke is not obvious, switches to vacuum, is evacuated to 30Pa; At 310 ℃ of reactions 1 hour, cooling discharge.Discharging 9.8kg records logarithmic viscosity number 4.6 altogether.
Embodiment 3:
The nylon oligomer 10kg that will contain dust joins and carries out solid-phase tack producing in the 50L rotary drum, and wherein particle diameter is greater than the material 8kg of 50um, and particle diameter is less than the material 2kg of 50um; Get into the logical nitrogen of pipe from nitrogen, rotate rotary drum, be warming up to 230 ℃; Smoke is not obvious, switches to vacuum, is evacuated to 25Pa; At 300 ℃ of reactions 1 hour, cooling discharge.Discharging 9.8kg records logarithmic viscosity number 2.4 altogether.
Embodiment 4:
The liquid crystal oligomer 10kg that will contain dust joins and carries out solid-phase tack producing in the 50L rotary drum, and wherein particle diameter is greater than the material 9.5kg of 50um, and particle diameter is less than the material 0.5kg of 50um; From the logical nitrogen of nitrogen air inlet pipe, rotate rotary drum, be warming up to 250 ℃; Smoke is not obvious, switches to vacuum, is evacuated to 35Pa; At 320 ℃ of reactions 1 hour, cooling discharge.Discharging 9.7kg records logarithmic viscosity number 4.5 altogether.
Comparative Examples 1:
The high-temperature nylon oligomer 10kg that will contain dust joins and carries out solid-phase tack producing in the 50L rotary drum, and wherein particle diameter is greater than the material 9kg of 50um, and particle diameter is less than the material 1kg of 50um; Be evacuated to 30Pa, rotate rotary drum, drop to 500Pa when temperature rises to 180 ℃ of vacuum; Cooling discharge, its colour changed into yellow.
Comparative Examples 2:
The high-temperature nylon oligomer 10kg that will contain dust sieves; Wherein particle diameter is greater than the material 9kg of 50um, and particle diameter is less than the material 1kg of 50um, particle diameter joined greater than the material of 50um carry out solid-phase tack producing in the rotary drum; Be evacuated to 30Pa; Rotate rotary drum, be warming up to 260 ℃ of reactions 6 hours, cooling discharge.Discharging 8.9kg records relative viscosity 2.3 altogether.
The method of testing of the relative viscosity of high-temperature nylon is:
The viscosimeter power switch is opened, and opened exact constant temperature groove, kind of refrigeration cycle groove switch, and the temperature control shelves are transferred to 25 ℃.Make viscosity test tank temperature stabilization at 25 ± 0.02 ℃ (opening device constant temperature in advance), carry out following operation behind the constant temperature:
A. blank testing (solvent) flow time: the concentrated sulfuric acid is injected viscosimeter (liquid level has requirement in the viscosity test method in the middle of two graduation marks); Then viscosimeter is put into the tank of constant temperature (assembling by the instrument instructions for use), with the about 30min of viscosimeter constant temperature in tank.Begin test then, select test relative viscosity I during setting.Record blank time t1.
B. test sample (solution) flow time: by the method test solution flow time t2 and the record of top blank testing.
Again t2 is got final product divided by t1.
The method of testing of the logarithmic viscosity number of liquid crystal is following:
Measuring concentration at 60 ℃ deuteriums in for Pentafluorophenol is the reduced inherent viscosity η of the liquid crystal of 0.1g/dl
Inhη
Inh=[ln (t
1/ t
0)]/C; Wherein, η
InhExpression reduced inherent viscosity (dl/g), t
0The flushing time (sec) of expression solvent, t
1The flushing time (sec) of expression sample solution, C representes the concentration (g/dl) of sample solution.
The said determination scheme is carried out mensuration as a result, and its result shows, adopts this agitated reactor to simplify operation, has reduced cost, has improved yield.And the little molecule of few absorption in the vacuum-pumping tube, can reduce cost of equipment maintenance greatly like this.
Claims (10)
1. a production has been prone to the agitated reactor of the material of powder in course of reaction; Its rotary drum (1) one end has charge door (2), and the other end has a manhole (3), the outer side joint rotating ring of rotary drum (1) (11); Inner turnover tracheae connects stationary ring (12); It is characterized in that: a vacuum-pumping tube (5) stretches into rotary drum (1) top, and its other end connects vavuum pump (10), and nitrogen air inlet pipe (4) stretches into rotary drum (1) bottom can be to rotary drum (1) delivered inside nitrogen.
2. a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder according to claim 1 is characterized in that a vacuum flap (6) is arranged on the mouth of pipe of vacuum-pumping tube (5).
3. a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder according to claim 1 is characterized in that the input of nitrogen air inlet pipe (4) is equipped with a valve (7).
4. a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder according to claim 1 is characterized in that, between vacuum-pumping tube (5) and the vavuum pump (10) cyclone separator (8) is housed.
5. a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder according to claim 1 is characterized in that, between vacuum-pumping tube (5) and the vavuum pump (10) cold-trap (9) is housed.
6. a kind of agitated reactor of producing the material that in course of reaction, has been prone to powder according to claim 1; It is characterized in that; In the rotary drum (1), the mouth of pipe of nitrogen air inlet pipe (4) is positioned at rotary drum (1) bottom, and vacuum-pumping tube (5) mouth of pipe is positioned at rotary drum (1) top.
7. prepare the said method that in course of reaction, has been prone to the material of powder of claim 1-6; It is characterized in that; The oligomer that will contain dust joins and carries out solid-phase tack producing in the rotary drum; Earlier logical high pure nitrogen is reacted to oligomer and discharges little molecule no longer in a large number, is evacuated to reaction to said viscosity below the 80pa again.
8. according to the said method that is prepared in the material that has been prone to powder in the course of reaction of claim 7, it is characterized in that, the particle diameter of oligomer greater than the material of 50um more than 90%.
9. according to the said method that is prepared in the material that has been prone to powder in the course of reaction of claim 7, it is characterized in that having a large amount of hanging down to adopt logical nitrogen tackify when molecules produce early stage in the solid-phase tack producing reaction.
10. according to the said method that is prepared in the material that has been prone to powder in the course of reaction of claim 7, it is characterized in that the low molecule that produces in the solid-phase tack producing reaction later stage adopts more after a little while and vacuumizes tackify.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102634313A CN102380336A (en) | 2011-09-07 | 2011-09-07 | Reactor for producing material easy to produce powder, and preparation method of the material |
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| CN2011102634313A CN102380336A (en) | 2011-09-07 | 2011-09-07 | Reactor for producing material easy to produce powder, and preparation method of the material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108213630A (en) * | 2016-12-12 | 2018-06-29 | 张跃 | It is a kind of to carry out the soldering system for heating/cooling down by medium of gas |
| CN112358611A (en) * | 2020-11-02 | 2021-02-12 | 万华化学集团股份有限公司 | Preparation method and application of semi-aromatic high-temperature-resistant nylon powder |
Citations (8)
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|---|---|---|---|---|
| CN2132136Y (en) * | 1992-05-09 | 1993-05-05 | 杨天泽 | Stickness strengthening of solid polyester stock and vacuum desiccating drum |
| US5603567A (en) * | 1995-02-17 | 1997-02-18 | Blentech Corporation | Coaxial cryogenic injection system |
| CN101492534A (en) * | 2008-12-26 | 2009-07-29 | 金发科技股份有限公司 | Process for preparing semi-aromatic polyamides |
| CN101503512A (en) * | 2009-03-03 | 2009-08-12 | 金发科技股份有限公司 | Semi-aromatic polyamide and preparation thereof |
| CN101525434A (en) * | 2009-04-08 | 2009-09-09 | 株洲时代新材料科技股份有限公司 | Basic magnesium sulfate whisker reinforced modified reaction injection nylon composite material and preparation method thereof |
| CN201434579Y (en) * | 2009-08-28 | 2010-03-31 | 金发科技股份有限公司 | High vacuum rotary drum cooling device for drying and tackifying polymer solid material |
| CN102079869A (en) * | 2010-12-20 | 2011-06-01 | 金发科技股份有限公司 | Preparation method of liquid crystal nylon alloy |
| CN202238022U (en) * | 2011-09-07 | 2012-05-30 | 金发科技股份有限公司 | Reaction kettle for producing material easily powdered in reaction process |
-
2011
- 2011-09-07 CN CN2011102634313A patent/CN102380336A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2132136Y (en) * | 1992-05-09 | 1993-05-05 | 杨天泽 | Stickness strengthening of solid polyester stock and vacuum desiccating drum |
| US5603567A (en) * | 1995-02-17 | 1997-02-18 | Blentech Corporation | Coaxial cryogenic injection system |
| CN101492534A (en) * | 2008-12-26 | 2009-07-29 | 金发科技股份有限公司 | Process for preparing semi-aromatic polyamides |
| CN101503512A (en) * | 2009-03-03 | 2009-08-12 | 金发科技股份有限公司 | Semi-aromatic polyamide and preparation thereof |
| CN101525434A (en) * | 2009-04-08 | 2009-09-09 | 株洲时代新材料科技股份有限公司 | Basic magnesium sulfate whisker reinforced modified reaction injection nylon composite material and preparation method thereof |
| CN201434579Y (en) * | 2009-08-28 | 2010-03-31 | 金发科技股份有限公司 | High vacuum rotary drum cooling device for drying and tackifying polymer solid material |
| CN102079869A (en) * | 2010-12-20 | 2011-06-01 | 金发科技股份有限公司 | Preparation method of liquid crystal nylon alloy |
| CN202238022U (en) * | 2011-09-07 | 2012-05-30 | 金发科技股份有限公司 | Reaction kettle for producing material easily powdered in reaction process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108213630A (en) * | 2016-12-12 | 2018-06-29 | 张跃 | It is a kind of to carry out the soldering system for heating/cooling down by medium of gas |
| CN112358611A (en) * | 2020-11-02 | 2021-02-12 | 万华化学集团股份有限公司 | Preparation method and application of semi-aromatic high-temperature-resistant nylon powder |
| CN112358611B (en) * | 2020-11-02 | 2022-07-12 | 万华化学集团股份有限公司 | Preparation method and application of semi-aromatic high-temperature-resistant nylon powder |
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Application publication date: 20120321 |