CN102807631A - Pipeline-type continuous polymerization reaction method - Google Patents
Pipeline-type continuous polymerization reaction method Download PDFInfo
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- CN102807631A CN102807631A CN2012102900091A CN201210290009A CN102807631A CN 102807631 A CN102807631 A CN 102807631A CN 2012102900091 A CN2012102900091 A CN 2012102900091A CN 201210290009 A CN201210290009 A CN 201210290009A CN 102807631 A CN102807631 A CN 102807631A
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Abstract
The invention discloses a pipeline-type continuous polymerization reaction method. The pipeline-type continuous polymerization reaction method comprises the following steps: A, respectively placing a raw material, a catalyst and an additive into a premixing tank set, a catalyst tank set and an additive tank set for uniformly mixing; B, inputting a mixed solution in the premixing tank set and a mixed solution in the catalyst tank set to a pipeline-type reactor for reacting to obtain a reaction solution, and heating the mixed solution which is just input to the reaction temperature; C, enabling the reaction solution to flow in the pipeline-type reactor and be subjected to polymerization reaction, wherein the flow speed of the reaction solution is not more than the quotient result of the pipeline length and the required reaction time; and D, finishing the polymerization reaction of the reaction solution before the reaction solution enters into the tail section of the pipeline-type reactor, cooling and adding the additive for pH and viscosity adjustment after the reaction solution enters into the tail section of the pipeline-type reactor, and directly outputting a polymer after uniformly mixing the additive through a discharge hole of the pipeline-type reactor. According to the pipeline-type continuous polymerization reaction method, the design of the conventional reaction kettle is changed into a pipeline-type design, so that the difficult problem of heat radiation is solved and the output is increased at the same time.
Description
Technical field
The present invention has designed a kind of brand-new continous way polymerization technology flow process.
Background technology
In the national economy life, many type materials derive from macromolecular polymerization reaction.With regard to liquid polymerization, just divide solution polymerization, suspension polymerization and letex polymerization.Building trade the used pressure-sensitive adhesive of used carpenter's glue, the adhesive article industry of a large amount of rubber-emulsion paint, woodworkings of using, weave used shaping glue of industry and print thickener etc., all be the product of polyreaction.In order to enhance productivity, reduce cost of labor and energy consumption, the deisgn approach of reaction kettle is in bigger volume in the big production of industry.But because technical process never changed, all effort have all run into bottleneck.The reaction unit of old-fashioned design is three external members basically: i.e. premix groove (or being referred to as emulsifying tank, tempering tank etc.), reaction kettle (or being referred to as reactive tank), neutralizing well (or being referred to as to adjust groove).The starting material monomer of promptly filling a prescription and being selected for use pumps in proportion in the premix groove and mixes or emulsification, in reactive tank, adds buffered soln, is heated to the polymerization temperature of selected raw material, adds seed mother liquor and initiator then, starts polyreaction.After polyreaction started, owing to be thermopositive reaction, through interlayer or the logical cooling water control temperature of reaction of coil pipe, liquid and initiator solution in the premix groove dripped simultaneously, adopted continuously or semi continuous (intermittent type or be referred to as sectional) dropping.Until all dropwising, be incubated for some time then, after question response is complete, be discharged to the neutralizing well cooling, adjust potential of hydrogen again and add other additives, the back packing stirs.The early response kettle amasss at 3～5 cubic metres, progressively is extended to 10～15 cubic metres, in recent years, because the progress of electromechanics and material; The reaction kettle volume expands to about 35 cubic metres, has just run into bottleneck, and it is not that the reaction kettle volume can not amplify; But go when amplifying again, reaction heat can't in time be derived, owing to be the radiating mode that adopts the logical water coolant of interlayer; The reaction kettle volume is big more, and the center is just far away more from the distance of still wall, and the reaction heat of central position just is difficult for being derived.Even the premix groove can be accomplished the proportioning raw materials pre-mixing that tolerance range is very high, but temperature can not control well, and then the quality of reactant is just unstable, so up to the present, maximum both at home and abroad reaction kettle just between 35～40 cubic metres, has or else enlarged.In addition, current batch (promptly a still is one batch) mode of production after the raw material in the premix groove dropwises, must be incubated for some time, lets its complete reaction.In other words; Soaking time is exactly that this polyreaction began to the time of accomplishing; And the previous reactant that drips is accomplished polymerization already, does not accomplish reaction and necessary the wait but be limited to last dropping thing, accomplishes polyreaction up to the total overall reaction thing and could press a batch discharging; So, production efficiency is except that improving through strengthening batch output again.
Summary of the invention
Problem to be solved by this invention is; Deficiency to above-mentioned technology; Designing a kind of duct type successive polymerization reaction method, is to overturn the formula thinking, and it becomes traditional reaction kettle into the duct type design; Neutralizing well also can be cancelled simultaneously, only reserves one section at extraction line and is used to adjust potential of hydrogen and adds other material.It has solved a heat radiation difficult problem, improves quantum of output simultaneously.
The technical scheme that the present invention is adopted for its problem of solution is:
Duct type successive polymerization reaction method is characterized in that may further comprise the steps:
A, elder generation put into premix groove group, catalyst tank group and additive tank group respectively with raw material, catalyzer and additive and mix;
B, the mixed solution in premix groove group, the catalyst tank group is inputed to react in the pipeline reactor make it become reaction solution again, the mixed solution of firm entering is heated to temperature of reaction;
C, reaction solution flow in pipeline reactor and carry out polyreaction, its velocity of flow smaller or equal to duct length divided by the essential reaction times;
D, reaction solution get into preceding oneself the completion polyreaction of answering of rear of pipeline reactor; Promptly cool off behind the entering rear and add additive and carry out adjustment of acid degree of subtracting and viscosity adjustment, the polymkeric substance after additive mixes is directly exported from the discharge port of pipeline reactor.
In the present invention, be placed with motor and whipping appts in premix groove group, catalyst tank group and/or the additive tank group described in the A step.
In the present invention, premix groove group, catalyst tank group and/or the additive tank group described in the A step is made up of with parallel way the tempering tank more than two or two.
In the present invention, the pipeline reactor described in the B step comprises airtight body, is provided with interceptor structure or dynamic stirring structure that reaction solution is fully reacted in the body.
In the present invention, the periphery of the pipeline reactor described in the B step is provided with the water-cooled temperature control system in order to the control internal temperature.
The invention has the beneficial effects as follows: 1, reaction solution of the present invention is in pipeline, to flow, and reaction continues to carry out, because initiate reaction solution does not disturb in the reaction of carrying out, so discharging time just can shift to an earlier date greatly.When 2, reaction starts, only need a small amount of reaction solution of leading portion (just having got into the reactor drum part) is heated, after the reaction beginning, heat release, hot water is back to the leading portion heat supply after the heat exchange, guarantees that reaction continues to carry out.3, owing to adopt the hermetic type pipeline reactor, clear jar of trouble having avoided old-fashioned batch of production to bring.Old-fashioned method production, after batch of completion, the reaction kettle of unstowing, polymkeric substance residual on the still wall is accumulated thickening again and again, seriously hinders heat exchange, so after producing several batches, must steep stove (high temperature alkali soaks cleaning), to guarantee radiating effect.4, the present invention can carry out full-automatic design fully, i.e. batching in premix groove group, catalyst tank group, the additive tank group, and optional automatic metering system, batching is accomplished the back stirring, goes into pipeline reactor with the pump of constant delivery type feeding.5, the self-reacting device cooperation is also equipped in the outer water-cooled temperature adjustment of reactor drum, can accomplish accurate temperature controller, makes quality product reach the most stable.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
Fig. 1 is the structural representation of present embodiment;
Fig. 2 is the structural representation of lune interceptor pipeline reactor;
Fig. 3 is the structural representation of flight interceptor pipeline reactor;
Fig. 4 is the structural representation of dynamic stirring formula pipeline reactor;
Fig. 5 is the structural representation of another kind of dynamic stirring formula pipeline reactor.
Embodiment
With reference to Fig. 1, the duct type successive polymerization reaction method that present embodiment provided may further comprise the steps:
A, elder generation put into premix groove group, catalyst tank group and additive tank group respectively with raw material, catalyzer and additive and mix; The volume of premix groove group, catalyst tank group and/or additive tank group can be increased to motor and whipping appts to greatest extent, also can adopt the mode of a plurality of parallel connections of smaller size smaller, decides according to the place size fully.When it adopts the mode of a plurality of parallel connections, can realize uninterrupted formula continuous production, promptly open second groove after a premix groove blowing finishes, first groove pan feeding again mixes subsequent use.The principle of work of catalyst tank group and additive tank group also together.Premix groove group need not heat, and key is to mix.
B, the mixed solution in premix groove group, the catalyst tank group is inputed to react in the pipeline reactor make it become reaction solution again; The periphery of pipeline reactor is provided with the water-cooled temperature control system in order to the control internal temperature; The water-cooled temperature control system cooperates with self-reacting device; Can accomplish accurate temperature controller, make quality product reach the most stable.When reaction starts, only need a small amount of reaction solution of leading portion (just having got into the reactor drum part) is heated, after the reaction beginning, heat release, hot water is back to the leading portion heat supply after the heat exchange, guarantees that reaction continues to carry out.Establish interceptor in the pipeline reactor cylindraceous to increase reaction solution circulation contact tube wall, so that reaction heat is in time derived.But big caliber reactor drum design motivation whipping appts.When reaction solution gets into pipeline reactor, add initiator solution in proportion simultaneously, mixing under the effect of interceptor or under the dynamic stirring effect.
C, reaction solution flow in pipeline reactor and carry out polyreaction, and the reaction solution flow control is relevant with the pipeline reactor caliber, and is relevant with duct length.Its key point will satisfy the reaction times exactly.For example: when caliber was 100cm, flow velocity was 1.0m/min, and pipe range is designed to 120 meters, and promptly the reaction times is 2 hours, and then flow is 0.785 cubic meters per minute.Then hourly output can reach more than 45 cubic metres.If needing controlling reaction time is 4 hours, then flow reduces by half, and hourly output also can reach about 23 cubic metres.The general flow velocity that adopts is fast, and long more helping of pipeline dispels the heat and mix.For example adopt 6 to be in charge of (152.4mm internal diameter), 2 meters/minute of flow velocitys react 2 hours meters, and then duct length needs 240 meters, and the design of can making a circulation then per hour can be produced 4.38 cubic metres of products.If large-scale professional enterprise, the pipeline reactor caliber can reach 2 meters, and length can reach hundreds of rice, and when Quan Zihua produced, hourly output can reach more than hundred tons.
The length of D, pipeline reactor cooperates with flow velocity, can make just to react completely, and gets into the rear cooling of pipeline reactor then, and adds additive, and the rear of pipeline reactor promptly mixes after flowing out, directly goes up the packing wire wrapping.In the present invention, pipeline reactor rear design additive adds inlet, when adopting big caliber reactor drum, can reserve and not hold the mixing tank of one to two dynamic stirring station as additive most, gets final product discharging after the mixing.
In the present invention, the design of pipeline reactor can be following several kinds of modes:
(1). as shown in Figure 2, lune interceptor pipeline reactor, this pipeline reactor are arranged at intervals with a plurality of semi-moon shaped interceptors, to increase reaction solution circulation contact tube wall, so that reaction heat is in time derived.
(2). as shown in Figure 3, flight interceptor pipeline reactor, this pipeline reactor are arranged at intervals with the flaky interceptor of a plurality of spirals.
(3). like Fig. 4, shown in 5, dynamic stirring formula pipeline reactor is arranged at intervals with a plurality of dynamic stirring structures in this pipeline reactor, to strengthen mixing uniformity, is particularly useful for the reactor drum of big caliber.As shown in Figure 5, the bottom of each dynamic stirring structure can be connected with letdown tank, and letdown tank is provided with switch-valve, when needs cleaning dynamic stirring structure, only need open switch-valve the discharge of the waste in the dynamic stirring structure is got final product.
Certainly, the present invention is except above-mentioned embodiment, and other equivalent technical solutions also should be within its protection domain.
Claims (5)
1. duct type successive polymerization reaction method is characterized in that may further comprise the steps:
A, elder generation put into premix groove group, catalyst tank group and additive tank group respectively with raw material, catalyzer and additive and mix;
B, the mixed solution in premix groove group, the catalyst tank group is inputed to react in the pipeline reactor make it become reaction solution again, the mixed solution of firm entering is heated to temperature of reaction;
C, reaction solution flow in pipeline reactor and carry out polyreaction, its velocity of flow smaller or equal to duct length divided by the essential reaction times;
D, reaction solution get into preceding oneself the completion polyreaction of answering of rear of pipeline reactor; Promptly cool off behind the entering rear and add additive and carry out adjustment of acid degree of subtracting and viscosity adjustment, the polymkeric substance after additive mixes is directly exported from the discharge port of pipeline reactor.
2. duct type successive polymerization reaction method according to claim 1 is characterized in that: be placed with motor and whipping appts in premix groove group, catalyst tank group and/or the additive tank group described in the A step.
3. duct type successive polymerization reaction method according to claim 1 is characterized in that: premix groove group, catalyst tank group and/or additive tank group described in the A step are made up of with parallel way the tempering tank more than two or two.
4. duct type successive polymerization reaction method according to claim 1, it is characterized in that: the pipeline reactor described in the B step comprises airtight body, is provided with interceptor structure or dynamic stirring structure that reaction solution is fully reacted in the body.
5. duct type successive polymerization reaction method according to claim 1 is characterized in that: the periphery of the pipeline reactor described in the B step is provided with the water-cooled temperature control system in order to the control internal temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408680A (en) * | 2013-08-27 | 2013-11-27 | 北京化工大学 | Energy-saving and high-efficiency self-cleaning polymerization process |
| CN103641142A (en) * | 2013-11-04 | 2014-03-19 | 东北大学设计研究院（有限公司） | Desilicication method for whole pipeline heating reaction of fly ash |
| CN103933921A (en) * | 2014-04-18 | 2014-07-23 | 盘锦万通科工贸有限公司 | Device and method for producing high-molecular polymer |
| CN105542080A (en) * | 2015-12-31 | 2016-05-04 | 广东工业大学 | Method for preparing petroleum resin in microreactor |
| CN114752015A (en) * | 2022-03-30 | 2022-07-15 | 安徽凯泽新材料有限公司 | Tubular continuous production process of butyronitrile latex |
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| CN1279693A (en) * | 1997-10-31 | 2001-01-10 | 奥格尼斯公司 | Continuous bulk polymerization process |
| CN1863822A (en) * | 2004-01-09 | 2006-11-15 | 罗姆两合公司 | Method for the continuous production of melt polymers in a tubular reactor |
| CN101148413A (en) * | 2007-09-29 | 2008-03-26 | 吴兆立 | Modification for high-pressure pipe reaction system of ethanolamine production |
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2012
- 2012-08-15 CN CN2012102900091A patent/CN102807631A/en active Pending
Patent Citations (4)
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| CN1265680A (en) * | 1997-08-05 | 2000-09-06 | 约翰逊商业贸易公司 | Process for producing hyperbranched polymers |
| CN1279693A (en) * | 1997-10-31 | 2001-01-10 | 奥格尼斯公司 | Continuous bulk polymerization process |
| CN1863822A (en) * | 2004-01-09 | 2006-11-15 | 罗姆两合公司 | Method for the continuous production of melt polymers in a tubular reactor |
| CN101148413A (en) * | 2007-09-29 | 2008-03-26 | 吴兆立 | Modification for high-pressure pipe reaction system of ethanolamine production |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408680A (en) * | 2013-08-27 | 2013-11-27 | 北京化工大学 | Energy-saving and high-efficiency self-cleaning polymerization process |
| CN103641142A (en) * | 2013-11-04 | 2014-03-19 | 东北大学设计研究院（有限公司） | Desilicication method for whole pipeline heating reaction of fly ash |
| CN103641142B (en) * | 2013-11-04 | 2015-10-28 | 东北大学设计研究院（有限公司） | A kind of desilication method of full canalization reacting by heating of flyash |
| CN103933921A (en) * | 2014-04-18 | 2014-07-23 | 盘锦万通科工贸有限公司 | Device and method for producing high-molecular polymer |
| CN105542080A (en) * | 2015-12-31 | 2016-05-04 | 广东工业大学 | Method for preparing petroleum resin in microreactor |
| CN105542080B (en) * | 2015-12-31 | 2018-09-18 | 广东工业大学 | A kind of method that Petropols are prepared in microreactor |
| CN114752015A (en) * | 2022-03-30 | 2022-07-15 | 安徽凯泽新材料有限公司 | Tubular continuous production process of butyronitrile latex |
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Effective date of registration: 20121227 Address after: 529300 Guangdong city of Jiangmen province Kaiping City second (Cangcheng) Industrial Park District No. 8 eight Applicant after: KAIPING QIYU ADHESIVE PRODUCTS TECHNOLOGY CO., LTD. Address before: Guangdong province Foshan city Chancheng District 528000 room 402 No. 87 Cheng Feng Li Applicant before: Luo Jier |
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