CN102690374A - Method for comprehensively drying liquid rubber and drying device - Google Patents
Method for comprehensively drying liquid rubber and drying device Download PDFInfo
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- CN102690374A CN102690374A CN2012101803018A CN201210180301A CN102690374A CN 102690374 A CN102690374 A CN 102690374A CN 2012101803018 A CN2012101803018 A CN 2012101803018A CN 201210180301 A CN201210180301 A CN 201210180301A CN 102690374 A CN102690374 A CN 102690374A
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Abstract
The invention provides a method for comprehensively drying liquid rubber. The method comprises the following steps of: 1) concentrating; and 2) performing thin film evaporation. The method for comprehensively drying the liquid rubber is suitable for drying the liquid rubber with both low viscosity and high viscosity, particularly the liquid rubber of which a liquid rubber solution or emulsion is low in concentration and high in solvent content, and the final product is high in viscosity. By adopting the drying device with a special structure and a combined mode, so that the drying efficiency and the treatment amount of the liquid rubber can be improved greatly, a liquid rubber product with qualified volatile matter can be obtained in a short period of time, and the residence time of the liquid rubber at high temperature can be reduced greatly; and therefore, the change of the performance and appearance of the liquid rubber remained at high temperature for a long time can be avoided.
Description
Technical field
The present invention relates to a kind of comprehensive drying method and drying installation of fluid rubber.
Background technology
Fluid rubber is meant that number-average molecular weight is the thick flowable liquids below 100000, and its major advantage is: easy handling, and available casting, injection machine-shaping, equipment is simple, easy construction; Can produce various rubber products from rubber overshoes, mechanicals to tire etc.; The processing aid that rubber industry is the best is like softening agent, tenderizer, cocuring agent, properties-correcting agent etc.; The softening agent of plastics industry; The embedding agent of electronic industry, coating-forming agent; And asphalt modifier.In addition, fluid rubber also can be widely used in makes various coating such as protective system, low thermo-paint, electrical insulating coating, water soluble paint and electrophoretic paint etc., has advantages such as tough and tensile, shock resistance.Especially big as be more suitable for as the Rubber processing softening agent greater than 10000 the time when the fluid rubber molecular weight; This softening agent can be participated in the sulfuration of rubber; Thereby can improve Rubber processing and physicals, reduce rubber and give birth to heat and rolling resistance, improve the rubber over-all properties.
Fluid rubber solution or emulsion adopt heating usually or carry out drying with the method that vacuumizes solvent in the system of removing; Volatile content is low more good more in the fluid rubber of dry back; Aspects such as mixed economy consider, require in the fluid rubber volatile content less than 0.5 weight % usually.Adopt with stirring tank exsiccant mode under vacuum condition in early days, though can be that volatile content meets the requirements, because reach 6-8 hour time of drying; Make fluid rubber in drying process, cause the crosslinked reaction of Denging; Cause molecular weight to increase, viscosity increases, the aging speed of expedite product; Directly influence performance of products and outward appearance, and energy consumption is higher, drying cycle long, can't realize operate continuously.Later stage is developed into the drying plant that adopts thin-film evaporator or special construction; Improved the drying efficiency of fluid rubber greatly; Reduced the fluid rubber residence time at high temperature, but up to the present used drying plant defectiveness still relates to a kind of sticky material exsiccant sticky material drying tower that is used for like patent CN88100708.0; This device comprises drying tower, condensing surface and vacuum pump; The column plate of symmetrical umbrella shape concave, convex shape is housed in drying tower, the emulsion of water content 63.2% in the time of can be charging, drying becomes the not thick product of water content; Can be removed to the fugitive constituent in the thick product below 1% simultaneously, cleaning cycle is long, simple in structure, easy to operate, cheap at interval for this tower.But be difficult to form thin liquid film when adopting this inventive method fluid rubber solution in this equipment, to flow; The evaporation area of unit volume fluid rubber solution is restricted; Get into the condensing surface on top because the iris action evaporable solvent of column plate is difficult through column plate when adopting this inventive method, influence the volatilization efficient of solvent, and the big drying that promptly contains the less fluid rubber of solvent of the only suitable original emulsion concentration of this invention (for example in the original emulsion moisture 63.2%); Volatile content in the dope that obtains is required relatively low (like volatile content < 1%; And volatile content of the present invention requires less than 0.5%), when solvent be more greatly the fluid rubber strength of solution more hour, the method through this invention is difficult to obtain the qualified fluid rubber of volatile content; Especially this inventive method only is fit to the drying of fluid rubber viscosity less than the 450PaS sticky material; When the viscosity of sticky material further increased, when for example viscosity was greater than 450PaS, flowability was relatively poor during the interstitial hole of sticky material through male and fomale(M&F); Interstitial hole is stopped up, influence the normal drying of fluid rubber; " gansu science and technology " 2004 the 20th the 10th phase of volume, " chemical science and technology " 2000 the 8th volume the 5th is interim have been introduced liquid divinyl rubber dry of terminal groups modification and has contrasted with the stir drying method; The drying efficiency that adopts thin-film evaporator is far above stirring tank; Material is residence time weak point at high temperature; Rerum natura and cosmetic variation are little, and fugitive constituent is qualified, but only mention in this method number-average molecular weight less than 4000, viscosity is less than the drying of 70Pas fluid rubber; Do not mention the drying of HMW, high viscosity liquid rubber; When being used for the high viscosity liquid rubber dryness, can causing thin-film evaporator outlet liquid-flow not smooth, thereby influence the normal operation of drying process; And this method only is fit to the drying that fluid rubber content in fluid rubber solution or the emulsion is more greatly relatively low as 50% left and right sides fluid rubber of solvent, is that solvent is difficult to make when bigger in the finished product volatile content qualified when fluid rubber content in fluid rubber solution or the emulsion is littler.
Summary of the invention
The object of the present invention is to provide a kind of comprehensive drying method and drying installation of fluid rubber; The present invention adopts the moisture eliminator of this inventive method and the drying that moisture eliminator combination method not only can satisfy the promptly middle low-viscosity (mobile) liquid rubber of middle lower molecular weight; And can satisfy the drying that HMW is a high viscosity liquid rubber; And drying efficiency is high; The fluid rubber solution that the array mode of this inventive method through different moisture eliminators can dry big concentration range simultaneously is dry, and can improve the treatment capacity of moisture eliminator.Adopt this inventive method not only can improve the drying efficiency of fluid rubber greatly; Reduce the energy consumption of fluid rubber drying process; And can significantly reduce the fluid rubber residence time at high temperature; Avoid the variation of fluid rubber performance and outward appearance, the fluid rubber volatile content that obtains simultaneously is lower.
The comprehensive drying method of fluid rubber provided by the invention, this method may further comprise the steps:
(1) be that fluid rubber solution or the emulsion of 5-60 % concentrates in temperature 50-100 ℃ scope with the fluid rubber weight content, the fluid rubber weight content is 70-95% in the liquid concentrator;
(2) concentrating liquid carries out thin film evaporation removal residual solvent in the step (1) in 50-150 ℃ of scope; The dispersion index that obtains number-average molecular weight and be 1000-100000, molecular weight is that 1.01-5, viscosity are the fluid rubber of 0.1-2000 Pas, and the fugitive constituent weight content is less than 0.5% in this fluid rubber.
In order to improve concentrated effect, be concentrated in pressure and be 0 and to-101.325kPa scope, carry out.
In order to improve the thin film evaporation effect, thin film evaporation is 0 to-101.325kPa scope, to carry out at pressure.
The drying installation of fluid rubber provided by the invention; It includes be connected thickener and thin-film evaporator; It is characterized in that: said thickener and thin-film evaporator inside top are provided with sparger and scum dredger; Thickener and thin-film evaporator outside top are communicated with solvent condenser, and the bottom of this solvent condenser is connected with the cooling solvent tank, in thin-film evaporator, also are provided with the whisking appliance of belt scraping plate.
Thickener is stirring tank or falling-film evaporator.
Said sparger is the disk that has concentric grooves and bulge-structure, is evenly equipped with rising solvent ventilating pit on its relief structure plane.
Whisking appliance bottom at belt scraping plate is equipped with stirring rake.
Said stirring rake is helical-ribbon type, anchor formula, frame or leaf formula.
Said solvent condenser also is connected with vacuum pump.
Drying means of the present invention not only is fit to the drying of liquid with small viscosity rubber; The drying that also is fit to the big fluid rubber of viscosity; Especially be fit to fluid rubber solution or emulsion concentration is less relatively, solvent is bigger, and the drying of the big fluid rubber of the finished product viscosity.Owing to adopted the drying installation with special construction and the array mode of this invention; Can improve the drying efficiency and the treatment capacity of fluid rubber greatly; Obtain the qualified fluid rubber product of fugitive constituent within a short period of time; Use this invention can significantly reduce the fluid rubber residence time at high temperature, thereby avoided the variation of performance and outward appearance under the long-time high temperature of fluid rubber.
Description of drawings
Fig. 1 is the structural representation of concentration technology in the drying installation of the present invention;
Fig. 2 is the structure of distributor synoptic diagram;
Fig. 3 is the structural representation of thin film evaporation technology in the drying installation of the present invention.
Embodiment
Embodiment described herein only is used for explanation and explains the present invention, is not limited to the present invention.
Embodiment 1
Rubber solutions to be dried is that the weight concentration that contains anti-aging agent is 10 %, and molecular weight is 30000, and MWD is 1.07 isoprene fluid rubber cyclohexane solution.
(1) rubber solutions to be dried gets into the thickener 1 among step (1) Fig. 1 with the speed of 800L/h; Thickener has concentrated sparger and concentrates scum dredger; Be installed in the disk that has concentric grooves 2-1 and bulge-structure 2-2 of the concentrated sparger 2 on the stir shaft 8; Groove is used for liquid to be carried, and is evenly equipped with rising solvent ventilating pit on the bulge-structure plane, and stir shaft 8 rotating speeds are 300r/min.Thickener 1 has chuck, heats to thickener through steam, is evacuated to-50kPa to system through concentrating vacuum pump 7, and the temperature in the thickener is 80 ℃.The isoprene fluid rubber solution that gets into thickener at first is evenly distributed on the wall of thickener through the sparger that rotates; The evaporable solvent is up; Get into concentrated solvent condensing surface 5 and concentrated solvent storage tank 6 through sparger, scum dredger, the descending outflow thickener of fluid rubber solution after concentrating gets into liquid concentrator storage tank 4.The fluid rubber weight content is 80 % in the liquid concentrator.
(2) the fluid rubber solution after concentrating gets into the thin-film evaporator 9 among Fig. 3 continuously from liquid concentrator storage tank 4, keeps the liquid level of liquid concentrator storage tank constant in the fill process, and the liquid flow rate that gets into thin-film evaporator is about 100L/h.The liquid concentrator that gets into thin-film evaporator at first flows on the thin-film evaporator wall through evaporation sparger 11; Effect at the scraper plate that is rotating 10 is distributed on the thin-film evaporator wall, and the solution on the wall used scraper plate to spread to very thin liquid film, and big viscous liquid rubber is selected for use fixedly scraper plate; Little viscous liquid rubber is selected to use movable scraping plate; Because the whisking appliance bottom has 4 oblique leaf oars of press-down type, tiltedly the angle of leaf oar and horizontal plane is 45 degree, makes this invention not only be fit to the drying of less viscous liquid rubber; The drying that also is fit to big viscous liquid rubber, the drying of especially suitable big viscous liquid rubber.The solvent of sending out in the Back stroke of thin film evaporation wall gets into evaporating solvent condensing surface 13 and evaporating solvent storage tank 14 through pervaporation sparger 11, evaporation scum dredger 12, and the descending outflow thin-film evaporator of dried fluid rubber gets into fluid rubber storage tank 16.Thin-film evaporator has chuck, heats to thin-film evaporator through steam, is evacuated to-90kPa to system through vacuum pump 15, and the temperature of vaporizer is 100 ℃.
The fugitive constituent weight content is 0.08 % in the liquid polyisoprene rubber that obtains after the drying, and outward appearance is near water white transparency, and number-average molecular weight is 30100, the dispersion index of molecular weight is 1.08.The viscosity of liquid polyisoprene rubber is about 90 Pas in the time of 38 ℃.
Comparative Examples 1
Getting 6000g is 10 % with the embodiment 1 identical weight concentration that contains anti-aging agent, and molecular weight is 30000, and MWD is 1.07 isoprene fluid rubber solution, adds in the stirring tank of 10L jacketed, and stirring tank is used steam heating.The stirring tank rotating speed is 500r/min, and the stirring tank temperature is 90 ℃.Vacuumize to stirring tank with vacuum pump, stirring tank vacuum tightness is about-90kPa, and be 4 hours time of drying.The fugitive constituent weight content is 1.5% in the liquid polyisoprene rubber that obtains after the drying, and the fluid rubber color is light yellow, and the number-average molecular weight of fluid rubber is 32500, and MWD is 1.22.Viscosity during 38 ℃ of liquid polyisoprene rubbers that obtains is about 93 Pas.
Comparative Examples 2
Like the method among the embodiment 1; The weight concentration that contains anti-aging agent is 10 %; Molecular weight is 30000, and MWD is that 1.07 isoprene fluid rubber solution does not get into thickener and concentrates and directly get into thin-film evaporator, and the volatile content that obtains liquid polyisoprene rubber is about 2.5%; Outward appearance is near water white transparency, and number-average molecular weight is 30200, the dispersion index of molecular weight is 1.09.Because the less polymers soln of concentration directly gets into thin-film evaporator; Cause unit volume solvent evaporation amount increase in the system, a large amount of evaporable solvents can be taken away partial polymer solution, not only can cause the waste of product; Prolonged operation also can be stopped up condenser system, shortens the device operational cycle.
Embodiment 2
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 10 %; Molecular weight is 30500, and MWD is 1.10 divinyl fluid rubber cyclohexane solution, and the volatile content of the liquid polybutadiene rubber that obtains is 0.07 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 30400, the dispersion index of molecular weight is 1.11.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 75 Pas.
Embodiment 3
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 10 %; Molecular weight is 31100, and MWD is 1.12 isoprene \ divinyl (weight ratio of isoprene and divinyl is 50:50) copolymer fluid body rubber hydrogenated gasoline (boiling range is 55-100 ℃) solution, and the volatile content of the liquid polybutadiene rubber that obtains is 0.08 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 31300, the dispersion index of molecular weight is 1.12.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 80 Pas.
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 10 %; Molecular weight is 60000, and MWD is 1.06 isoprene fluid rubber cyclohexane solution, and the volatile content of the liquid polybutadiene rubber that obtains is 0.10 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 59900, the dispersion index 1.08 of molecular weight.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 700 Pas.
Comparative Examples 3
With the rubber solutions to be dried among the embodiment 4; Carry out drying according to the method among the embodiment 1; Just whisking appliance is not installed in the bottom of film evaporator; The volatile content of the liquid polyisoprene rubber that obtains is 0.5 weight %, and outward appearance is near water white transparency, and number-average molecular weight is 60100, the dispersion index 1.07 of molecular weight.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 700 Pas.But the thin-film evaporator outlet is stopped up, cause irregular parking, influence the ordinary production of product.
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 20 %; Molecular weight is 20000, and MWD is 1.08 isoprene cyclohexane solution, and the volatile content of the liquid polyisoprene rubber that concentrating liquid obtains is 0.07 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 20200, the dispersion index 1.08 of molecular weight.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 45Pas.
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 30 %; Molecular weight is 10000, and MWD is 1.09 isoprene cyclohexane solution, and the volatile content of the liquid polyisoprene rubber that obtains is 0.06 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 9950, the dispersion index 1.10 of molecular weight.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 15Pas.
Method according to embodiment 1; Be that rubber solutions to be dried changes that to do the weight concentration that contains anti-aging agent be 40 %; Molecular weight is 5000, and MWD is 1.11 isoprene cyclohexane solution, and the volatile content of the liquid polyisoprene rubber that obtains is 0.05 weight %; Outward appearance is near water white transparency, and number-average molecular weight is 5000, the dispersion index 1.10 of molecular weight.The viscosity that the liquid polyisoprene rubber that obtains is 38 ℃ is about 3.5Pas.
According to the method for embodiment 1, just be evacuated to-50kPa to system through vacuum pump 7 in (1), the temperature in the thickener is 70 ℃.The fluid rubber weight content is 75 % in the liquid concentrator.(2) be evacuated to-90kPa to system through vacuum pump 15, the temperature of vaporizer is 110 ℃.The fugitive constituent weight content is 0.08 % in the liquid polyisoprene rubber that obtains after the drying, and outward appearance is near water white transparency, and number-average molecular weight is 30200, the dispersion index of molecular weight is 1.07.The viscosity of liquid polyisoprene rubber is about 90 Pas in the time of 38 ℃.
Embodiment 9
According to the method for embodiment 1, just be evacuated to-50kPa to system through vacuum pump 7 in (1), the temperature in the thickener is 90 ℃.The fluid rubber weight content is 85 % in the liquid concentrator.(2) be evacuated to-90kPa to system through vacuum pump 15, the temperature of vaporizer is 110 ℃.The fugitive constituent weight content is 0.08 % in the liquid polyisoprene rubber that obtains after the drying, and outward appearance is near water white transparency, and number-average molecular weight is 30600, the dispersion index of molecular weight is 1.08.The viscosity of liquid polyisoprene rubber is about 90 Pas in the time of 38 ℃.
Result's contrast through embodiment 1-9 and Comparative Examples 1-3; Can find out and adopt moisture eliminator of the present invention and moisture eliminator combination mode to carry out efficient drying the fluid rubber of different molecular weight, different viscosity, different solutions concentration; Especially can be less relatively to the original liquid rubber concentrations, fluid rubber efficient drying that the finished product viscosity is bigger; And drying efficiency is high, and fluid rubber outward appearance and structure are had no adverse effects.
Claims (9)
1. the comprehensive drying method of a fluid rubber, it is characterized in that: this method may further comprise the steps:
(1) be that fluid rubber solution or the emulsion of 5-60 % concentrates in temperature 50-100 ℃ scope with the fluid rubber weight content, the fluid rubber weight content is 70-95% in the concentrating liquid that obtains;
(2) concentrating liquid carries out thin film evaporation removal residual solvent in the step (1) in 50-150 ℃ of scope; The dispersion index that obtains number-average molecular weight and be 1000-100000, molecular weight is that 1.01-5, viscosity are the fluid rubber of 0.1-2000 Pas, and the fugitive constituent weight content is less than 0.5% in this fluid rubber.
2. the comprehensive drying method of fluid rubber according to claim 1 is characterized in that: the pressure that is concentrated in the step (1) is 0 to-101.325kPa scope, to carry out.
3. the comprehensive drying method of fluid rubber according to claim 1 is characterized in that: the thin film evaporation in the step (2) is 0 to-101.325kPa scope, to carry out at pressure.
4. the drying installation of a fluid rubber; It includes thickener and the thin-film evaporator that is connected; It is characterized in that: said thickener and thin-film evaporator inside top are provided with sparger and scum dredger; Thickener and thin-film evaporator outside top are communicated with solvent condenser, and the bottom of this solvent condenser is connected with the cooling solvent tank, in thin-film evaporator, also are provided with the whisking appliance of belt scraping plate.
5. the drying installation of fluid rubber according to claim 4, it is characterized in that: thickener is stirring tank or falling-film evaporator.
6. the drying installation of fluid rubber according to claim 4, it is characterized in that: said sparger is the disk that has concentric grooves and bulge-structure, is evenly equipped with rising solvent ventilating pit on its relief structure on the plane.
7. the drying installation of fluid rubber according to claim 4 is characterized in that: bottom the whisking appliance of belt scraping plate, stirring rake is installed.
8. the drying installation of fluid rubber according to claim 7, it is characterized in that: said stirring rake is helical-ribbon type, anchor formula, frame or leaf formula.
9. the drying installation of fluid rubber according to claim 4, it is characterized in that: said solvent condenser also is connected with vacuum pump.
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| CN2012101803018A CN102690374A (en) | 2012-06-04 | 2012-06-04 | Method for comprehensively drying liquid rubber and drying device |
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| CN2012101803018A CN102690374A (en) | 2012-06-04 | 2012-06-04 | Method for comprehensively drying liquid rubber and drying device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107551584A (en) * | 2017-09-15 | 2018-01-09 | 山西翔宇化工有限公司 | A kind of processing method of age resistor purification |
| CN108047357A (en) * | 2018-01-29 | 2018-05-18 | 山东贝隆杜仲生物工程有限公司 | A kind of eucommia ulmoides refined glue dries aftertreatment technology |
| CN108659147A (en) * | 2018-05-30 | 2018-10-16 | 海南省先进天然橡胶复合材料工程研究中心有限公司 | A kind of Heveatex physics dewatering |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107551584A (en) * | 2017-09-15 | 2018-01-09 | 山西翔宇化工有限公司 | A kind of processing method of age resistor purification |
| CN108047357A (en) * | 2018-01-29 | 2018-05-18 | 山东贝隆杜仲生物工程有限公司 | A kind of eucommia ulmoides refined glue dries aftertreatment technology |
| CN108659147A (en) * | 2018-05-30 | 2018-10-16 | 海南省先进天然橡胶复合材料工程研究中心有限公司 | A kind of Heveatex physics dewatering |
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Application publication date: 20120926 |