CN117003912A - Aromatic vinyl monomer-conjugated diene block copolymer and method for drying same - Google Patents
Aromatic vinyl monomer-conjugated diene block copolymer and method for drying same Download PDFInfo
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- CN117003912A CN117003912A CN202210469996.5A CN202210469996A CN117003912A CN 117003912 A CN117003912 A CN 117003912A CN 202210469996 A CN202210469996 A CN 202210469996A CN 117003912 A CN117003912 A CN 117003912A
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- 239000000178 monomer Substances 0.000 title claims abstract description 88
- 150000001993 dienes Chemical class 0.000 title claims abstract description 85
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 85
- 238000001035 drying Methods 0.000 title claims abstract description 69
- 229920001400 block copolymer Polymers 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000007603 infrared drying Methods 0.000 claims abstract description 36
- 229920001577 copolymer Polymers 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 14
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 24
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims description 12
- KAKZBPTYRLMSJV-UHFFFAOYSA-N butadiene group Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 9
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- VSKJLJHPAFKHBX-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical class CC(=C)C=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 VSKJLJHPAFKHBX-UHFFFAOYSA-N 0.000 claims description 2
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical class C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims description 2
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 10
- 208000005156 Dehydration Diseases 0.000 description 9
- 238000001125 extrusion Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000012790 adhesive layer Substances 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- -1 alkyl lithium Chemical compound 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/06—Treatment of polymer solutions
- C08F6/10—Removal of volatile materials, e.g. solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
- B29B13/065—Conditioning or physical treatment of the material to be shaped by drying of powder or pellets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sustainable Development (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention relates to the field of polymer post-treatment, and discloses an aromatic vinyl monomer-conjugated diene segmented copolymer and a drying method thereof. The method comprises the following steps: vacuum infrared drying is carried out on the aromatic vinyl monomer-conjugated diene segmented copolymer; the aromatic vinyl monomer-conjugated diene block copolymer obtained by drying has a water content of 0.8wt% or less. According to the method, the aromatic vinyl monomer-conjugated diene segmented copolymer colloidal particles are deeply dried by adopting a vacuum infrared drying method, so that the copolymer with qualified volatile content can be obtained at a lower temperature, the performance of the dried copolymer is ensured, the energy consumption can be obviously reduced, and the emission of tail gas to the environment is reduced.
Description
Technical Field
The invention relates to the field of polymer post-treatment, in particular to a method for drying an aromatic vinyl monomer-conjugated diene block copolymer and the dried aromatic vinyl monomer-conjugated diene block copolymer obtained by the method.
Background
The aromatic vinyl monomer-conjugated diene block copolymer is a polymer obtained by adding an aromatic vinyl monomer and a conjugated diene monomer through different sequential monomer addition modes. The aromatic vinyl monomer-conjugated diene segmented copolymer is a novel third-generation synthetic rubber with thermoplastic processability and elastomer mechanical properties, and according to different requirements of market application, a plurality of aromatic vinyl monomer-conjugated diene segmented copolymers with excellent performances and different brands can be prepared by changing the proportion of two monomers in the polymer, the molecular weight of the polymer, the molecular weight distribution and the structure of polymer chains. The modified asphalt is mainly used for modifying asphalt, shoemaking and adhesive making, and can be mixed with a plurality of materials, such as plasticizer, modifier, filler, other resin and the like. Such blending can vary the properties of the material, such as softening temperature, tackiness, cohesive bond strength and rigidity, depending on the needs of the particular application, and thus the aromatic vinyl monomer-conjugated diene block copolymer has a very wide range of applications.
The process for producing the aromatic vinyl monomer-conjugated diene block copolymer generally comprises the steps of compounding and metering an auxiliary agent, polymerizing, agglomerating, dehydrating, drying and the like. When a wet coagulation process is used to remove the solvent added during the polymerization, the water content of the coagulated block copolymer particles after washing is usually about 40 wt%. Even if extruded by an extruder, the aromatic vinyl monomer-conjugated diene block copolymer still has a water content of about 8wt% and cannot meet the standard that the volatile content required for the aromatic vinyl monomer-conjugated diene block copolymer is lower than 0.8 wt%. Therefore, a deep drying process is necessary.
In the prior art, the extruded and dehydrated aromatic vinyl monomer-conjugated diene block copolymer colloidal particles are subjected to deep drying by adopting expansion drying and a large amount of hot air fluidization drying so as to ensure that the volatile matters meet the quality requirements of the copolymer. When expansion drying is carried out, the first, second and third sections of the temperature of the dryer are controlled by steam, the operation temperature is higher, and particularly in the third section, the temperature is controlled to be about 150 ℃ to obtain the copolymer with qualified volatile content. Drying at this relatively high temperature tends to cause the copolymer to become tacky and clump, resulting in a thick layer of crumb on the conveyor, and eventually a large amount of floor glue, severely limiting the improvement in the yield of the aromatic vinyl monomer-conjugated diene block copolymer. In addition, since the colloidal particles after expansion drying are sticky, a large amount of hot air is needed to fluidize and dry the colloidal particles to obtain the block copolymer with qualified volatile components, a large amount of tail gas containing VOC is generated, and the environment is not protected.
Therefore, the existing drying method of the aromatic vinyl monomer-conjugated diene segmented copolymer needs to be optimized and improved, so that the quality of the aromatic vinyl monomer-conjugated diene segmented copolymer is not damaged as much as possible in the drying process, the energy consumption and the exhaust emission in the drying process are reduced, and the harmony and win-win of the quality of the copolymer and the environmental protection are realized.
Disclosure of Invention
The invention aims to solve the problems of low copolymer quality, high energy consumption required by drying and high exhaust emission generated in the drying process caused by high drying temperature in the prior art, and provides a method for drying an aromatic vinyl monomer-conjugated diene block copolymer and the aromatic vinyl monomer-conjugated diene block copolymer obtained by the method. According to the method, the aromatic vinyl monomer-conjugated diene segmented copolymer colloidal particles are deeply dried by adopting a vacuum infrared drying method, so that the copolymer with qualified volatile content can be obtained at a lower temperature, the performance of the dried copolymer is ensured, the energy consumption can be obviously reduced, and the emission of tail gas to the environment is reduced.
In order to achieve the above object, the first aspect of the present invention provides a method for drying an aromatic vinyl monomer-conjugated diene block copolymer, characterized by comprising: vacuum infrared drying is carried out on the aromatic vinyl monomer-conjugated diene segmented copolymer;
the aromatic vinyl monomer-conjugated diene block copolymer obtained by drying has a water content of 0.8wt% or less.
The second aspect of the present invention provides an aromatic vinyl monomer-conjugated diene block copolymer obtained by drying by the above method.
Through the technical scheme, the aromatic vinyl monomer-conjugated diene block copolymer and the drying method thereof provided by the invention have the following beneficial effects:
when the method for drying the aromatic vinyl monomer-conjugated diene block copolymer adopts a vacuum infrared drying technology to dry the aromatic vinyl monomer-conjugated diene block copolymer, the surface and the inside of the colloidal particle can be heated simultaneously due to the penetrating power of infrared rays, the transfer of a heat medium is not needed, the rapid temperature rise can be realized, the stable control of the temperature is easy, the heating effect with high efficiency and high uniformity is generated, and the high-quality copolymer with qualified volatile components is further obtained.
Further, the method for drying the aromatic vinyl monomer-conjugated diene segmented copolymer can be used for deeply drying colloidal particles, and can be used for obtaining the copolymer with qualified volatile content at a lower temperature, so that the dried copolymer has excellent mechanical properties.
Drawings
FIG. 1 is a flow chart showing a method for drying an aromatic vinyl monomer-conjugated diene block copolymer according to the present invention.
Description of the reference numerals
1 particles of an aqueous aromatic vinyl monomer-conjugated diene block copolymer; 2, extruding a dehydrator; 3, vacuum infrared drying box; 4 aromatic vinyl monomer-conjugated diene block copolymer.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The present invention provides, in a first aspect, a method for drying an aromatic vinyl monomer-conjugated diene block copolymer, characterized by comprising:
the water content of the para-aromatic vinyl monomer-conjugated diene block copolymer is 0.8wt% or less.
According to the invention, when the vacuum infrared drying technology is adopted to dry the aromatic vinyl monomer-conjugated diene segmented copolymer, the surface and the inside of the colloidal particle can be heated simultaneously due to the penetrating power of infrared rays, the transfer of a heat medium is not needed, the rapid temperature rise can be realized, the stable control of the temperature is easy, the heating effect with high efficiency and high uniformity is generated, and the high-quality copolymer with qualified volatile components is further obtained.
According to the present invention, the water content of the aromatic vinyl monomer-conjugated diene block copolymer obtained by drying is 0.6wt% or less.
According to the invention, the absolute operating pressure of the vacuum infrared drying is 1-20kPa.
In the present invention, the aromatic vinyl monomer-conjugated diene block copolymer is dried in the absolute operating pressure range, and the aromatic vinyl monomer-conjugated diene block copolymer having a satisfactory volatile content can be obtained at a low drying temperature.
Further, the absolute operating pressure of the vacuum infrared drying is 5-15kPa.
According to the invention, the operating temperature of the vacuum infrared drying is 30-80 ℃.
In the present invention, the aromatic vinyl monomer-conjugated diene block copolymer is dried at the above-mentioned operating temperature, and the deterioration of the quality of the aromatic vinyl monomer-conjugated diene block copolymer at high temperature can be avoided, thereby obtaining an aromatic vinyl monomer-conjugated diene block copolymer having excellent performance.
Further, the operating temperature of the vacuum infrared drying is 40-70 ℃.
According to the invention, the time of vacuum infrared drying is 0.2-0.9h.
In the present invention, the aromatic vinyl monomer-conjugated diene block copolymer is dried within the above-described time period, and the drying efficiency can be ensured, and a high-quality aromatic vinyl monomer-conjugated diene block copolymer can be obtained.
Further, the operating temperature of the vacuum infrared drying is 0.3-0.7h.
According to the invention, the power consumption of the vacuum infrared drying oven is 1-3kW/kg of pure polymer.
In the invention, the aromatic vinyl monomer-conjugated diene block copolymer is dried within the power consumption range, so that the drying efficiency and the quality of the dried product can be ensured.
Further, the power consumption of the vacuum infrared drying oven is 1.5-2.5kW/kg of pure polymer.
According to the present invention, the hard segment is provided by the aromatic vinyl monomer in an amount of 30 to 40wt% based on the total weight of the aromatic vinyl monomer-conjugated diene block copolymer; the soft segment is provided by the conjugated diene in an amount of 60 to 70wt%.
In the present invention, when the hard segment content provided by the aromatic vinyl monomer in the aromatic vinyl monomer-conjugated diene block copolymer satisfies the above range, the block copolymer is made to have excellent strength and elasticity.
In the present invention, the weight average molecular weight and the like of the aromatic vinyl monomer-conjugated diene block copolymer are not particularly limited, and various aromatic vinyl monomer-conjugated diene block copolymers having different weight average molecular weights in the prior art may be used.
In the present invention, the types of the aromatic vinyl monomer and the conjugated diene are not particularly limited, and may be aromatic vinyl monomers or conjugated dienes which are conventional in the art, for example, styrene, and the conjugated dienes may be butadiene and/or isoprene.
Further, the aromatic vinyl monomer-conjugated diene block copolymer is selected from at least one of styrene-butadiene-styrene block copolymer (SBS), hydrogenated styrene-butadiene-styrene block copolymer (SEBS), styrene-isoprene-styrene block copolymer (SIS), and hydrogenated styrene-isoprene-styrene block copolymer (SEPS).
According to the present invention, the aromatic vinyl monomer-conjugated diene block copolymer is derived from solution polymerization.
In the present invention, the polymerization method of the aromatic vinyl monomer-conjugated diene block copolymer is not particularly limited, and a solution polymerization method conventional in the art, for example, may be employed: the block copolymer with different hard segment and soft segment contents can be obtained by taking styrene, butadiene (or isoprene) as monomers, saturated straight-chain alkane or cycloalkane as solvent, and alkyl lithium as initiator to carry out copolymerization of the two monomers.
In the present invention, the polymerization system of the aromatic vinyl monomer-conjugated diene block copolymer is not particularly limited, and a continuous solution polymerization system or a batch solution polymerization system may be employed.
In the present invention, the conditions for the solution polymerization and the amounts of the aromatic vinyl monomer, conjugated diene, initiator and the like are not particularly limited, and the polymerization may be carried out in conventional amounts under the conditions of the solution polymer which are conventional in the art.
According to the invention, the method comprises the following steps:
s1, carrying out wet condensation and coarse dehydration on an aromatic vinyl monomer-conjugated diene block copolymer from solution polymerization to obtain aqueous copolymer particles;
s2, extruding and dehydrating the water-containing copolymer particles to obtain a preform;
and S3, drying the preform by vacuum infrared drying to obtain the aromatic vinyl monomer-conjugated diene segmented copolymer.
In the present invention, a large amount of solvent carried by the aromatic vinyl monomer-conjugated diene block copolymer from solution polymerization can be removed by wet coagulation.
In the present invention, the coarse dewatering treatment is not particularly limited, and the coarse dewatering treatment may be carried out on the aqueous colloidal particles by using a vibrating screen apparatus commonly used in the art, such as a linear vibrating screen, a reciprocating vibrating screen, a rotary vibrating screen, and the like.
In the present invention, the extrusion dehydration treatment is not particularly limited, and extrusion dehydration treatment of aqueous colloidal particles can be performed by using extruder equipment commonly used in the art, such as a single screw extruder, a twin screw extruder, a multi-screw extruder, etc.
In the invention, the volatile content in the preform obtained by rough dehydration treatment and extrusion dehydration treatment is about 10 wt%.
Referring to fig. 1, in one embodiment of the present invention, a method of drying an aromatic vinyl monomer-conjugated diene block copolymer comprises the steps of:
the aromatic vinyl monomer-conjugated diene random copolymer from solution polymerization is subjected to wet coagulation and coarse dehydration to obtain aqueous aromatic vinyl-conjugated diene block copolymer particles 1;
the aqueous aromatic vinyl-conjugated diene block copolymer particles 1 are subjected to extrusion dehydration treatment by an extrusion dehydrator 2 to obtain a preform;
and drying the preform by adopting a vacuum infrared dryer 3 to obtain the aromatic vinyl monomer-conjugated diene segmented copolymer 4.
The second aspect of the present invention provides an aromatic vinyl monomer-conjugated diene block copolymer obtained by drying by the above method.
In the present invention, the volatile content in the aromatic vinyl monomer-conjugated diene block copolymer is 0.8wt% or less, preferably 0.6wt% or less.
The present invention will be described in detail by examples.
The following examples and comparative examples each use a styrene-butadiene-styrene block copolymer as an aromatic vinyl monomer-conjugated diene block copolymer.
Styrene and butadiene are used as comonomers, cyclohexane is used as a solvent, butyl lithium is used as an initiator, solution polymerization is carried out in a kettle type polymerization reactor to obtain a styrene-butadiene-styrene block copolymer, the content of a hard segment provided by styrene is 35wt% and the content of a soft segment provided by butadiene is 65wt% based on the total weight of the styrene-butadiene-styrene block copolymer.
The tensile strength, elongation at break and permanent set of the vulcanizate were measured according to the methods described in GB/T528 standard.
In the following examples and comparative examples, other various raw materials were used from commercial sources unless otherwise specified.
In the following examples and comparative examples, the method for measuring the volatile content was an oven method unless otherwise specified.
Example 1
S1, carrying out wet condensation and coarse dehydration on a styrene-butadiene-styrene block copolymer from solution polymerization to obtain aqueous copolymer particles;
s2, in an extrusion dehydrator, carrying out extrusion dehydration treatment on the water-containing copolymer particles to obtain a preform, wherein the water content of the preform is 10wt%;
s3, drying the preform by vacuum infrared drying to obtain the styrene-butadiene-styrene block copolymer, wherein the vacuum infrared drying conditions are as follows: the absolute operating pressure was 5kPa, the operating temperature was 40℃and the time was 0.7h, the power consumption was 2kW/kg of pure polymer.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 2
Example 1 was substantially repeated, except that: in step S3, the operation time of vacuum infrared drying is 0.5h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 3
Example 1 was substantially repeated, except that: in step S3, the operation time of vacuum infrared drying is 0.3h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 4
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 10kPa, the drying temperature is 60 ℃, and the drying time is 0.7h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 5
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 10kPa, the drying temperature is 60 ℃, and the drying time is 0.5h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 6
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 10kPa, the drying temperature is 60 ℃, and the drying time is 0.3h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 7
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 15kPa, the drying temperature is 70 ℃, and the drying time is 0.7h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 8
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 15kPa, the drying temperature is 70 ℃, and the drying time is 0.5h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Example 9
Example 1 was substantially repeated, except that: in step S3, the absolute operating pressure of the vacuum infrared drying is 15kPa, the drying temperature is 70 ℃, and the drying time is 0.3h.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Comparative example 1
Example 1 was essentially repeated except that the vacuum infrared drying oven of example 1 was replaced with an expansion dryer with a power consumption of 2kW/kg of pure polymer. The first stage temperature of the expansion dryer is controlled to 80 ℃, the second stage temperature is controlled to 100 ℃, and the third stage temperature is controlled to 135 ℃.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
Comparative example 2
Example 1 was essentially repeated except that the vacuum infrared drying oven of example 1 was replaced with an expansion dryer with a power consumption of 4kW/kg of pure polymer, wherein the first stage temperature was controlled to 100 c, the second stage temperature was controlled to 125 c, and the third stage temperature was controlled to 145 c.
The water content and appearance quality of the styrene-butadiene-styrene block copolymer obtained by drying are shown in Table 1.
TABLE 1
| Moisture content (wt%) | Appearance quality of the product | |
| Example 1 | 0.53 | White and dry thoroughly |
| Example 2 | 0.56 | White and dry thoroughly |
| Example 3 | 0.58 | White and dry thoroughly |
| Example 4 | 0.47 | White and dry thoroughly |
| Example 5 | 0.49 | White and dry thoroughly |
| Example 6 | 0.51 | White and dry thoroughly |
| Example 7 | 0.42 | White and dry thoroughly |
| Example 8 | 0.45 | White and dry thoroughly |
| Example 9 | 0.47 | White and dry thoroughly |
| Example 10 | 0.58 | White and dry thoroughly |
| Example 11 | 0.57 | White and dry thoroughly |
| Example 12 | 0.62 | White and the adhesive layer surface has a few pinch points |
| Comparative example 1 | 1.0 | Yellowish, with a few pinch points on the surface and middle of the adhesive layer |
| Comparative example 2 | 0.9 | Yellowish, adhesive layer with surface and middle part of it |
As can be seen from the data in Table 1, according to the invention, when the extruded styrene-butadiene-styrene block copolymer colloidal particles are dried by adopting a vacuum infrared drying technology, the moisture in the colloidal particles can be removed as much as possible under the condition of lower temperature, so that the requirement of the product on the volatile content is realized; and the product is white and transparent from the appearance, and the phenomenon of clamping generation is not easy to occur in the drying process.
Test case
The aromatic vinyl monomer-conjugated diene block copolymer obtained by drying according to the drying method of examples and comparative examples was molded, and the physical and mechanical properties of the molded samples were tested, and the results are shown in Table 2.
The molding conditions include: the molding temperature is 155 ℃, the molding time is 20min, and the molding pressure is 3.5MPa.
TABLE 2
| Tensile Strength (MPa) | Elongation at break (%) | Permanent deformation at break (%) | |
| Example 1 | 25.3 | 762 | 41 |
| Example 2 | 25.1 | 760 | 41 |
| Example 3 | 24.9 | 756 | 42 |
| Example 4 | 26.1 | 771 | 39 |
| Example 5 | 25.7 | 764 | 39 |
| Example 6 | 25.4 | 762 | 40 |
| Example 7 | 26.9 | 785 | 36 |
| Example 8 | 26.6 | 778 | 37 |
| Example 9 | 26.1 | 771 | 39 |
| Example 10 | 24.9 | 756 | 42 |
| Example 11 | 24.8 | 756 | 42 |
| Example 12 | 24.5 | 751 | 43 |
| Comparative example 1 | 24.0 | 740 | 46 |
| Comparative example 2 | 24.1 | 745 | 44 |
As can be seen from the data shown in Table 2, the aromatic vinyl monomer-conjugated diene block copolymer (styrene-butadiene-styrene block copolymer) with qualified volatile content, which is obtained by adopting the vacuum infrared drying technology, has higher tensile strength and elongation at break and lower permanent deformation value, thus having better mechanical property.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (11)
1. A method of drying an aromatic vinyl monomer-conjugated diene block copolymer, the method comprising: vacuum infrared drying is carried out on the aromatic vinyl monomer-conjugated diene segmented copolymer;
the aromatic vinyl monomer-conjugated diene block copolymer obtained by drying has a water content of 0.8wt% or less.
2. The method according to claim 1, wherein the water content of the aromatic vinyl monomer-conjugated diene block copolymer obtained by drying is 0.6wt% or less.
3. A method according to claim 1 or 2, wherein the absolute operating pressure of the vacuum infrared drying is 1-20kPa, preferably 5-15kPa.
4. A method according to any one of claims 1-3, wherein the vacuum infrared drying is operated at a temperature of 30-80 ℃, preferably 40-70 ℃.
5. The method according to any one of claims 1-4, wherein the vacuum infrared drying is performed for a time of 0.2-0.9h, preferably 0.3-0.7h.
6. The method according to any of claims 1-5, wherein the vacuum infrared drying oven has a power consumption of 1-3kW/kg pure polymer, preferably 1.5-2.5kW/kg pure polymer.
7. The process according to any one of claims 1 to 6, wherein the hard segment is provided by the aromatic vinyl monomer in an amount of 30 to 40wt% and the soft segment is provided by the conjugated diene in an amount of 60 to 70wt%, based on the total weight of the aromatic vinyl monomer-conjugated diene block copolymer.
8. The method of any of claims 1-7, wherein the aromatic vinyl monomer-conjugated diene block copolymer, the aromatic vinyl monomer is styrene, and the conjugated diene is selected from butadiene and/or isoprene;
preferably, the aromatic vinyl monomer-conjugated diene block copolymer is selected from at least one of a styrene-butadiene-styrene block copolymer, a hydrogenated styrene-butadiene-styrene block copolymer, a styrene-isoprene-styrene block copolymer, and a hydrogenated styrene-isoprene-styrene block copolymer.
9. The method of any of claims 1-8, wherein the aromatic vinyl monomer-conjugated diene block copolymer is derived from solution polymerization.
10. The method according to any one of claims 1-9, wherein the method comprises the steps of:
s1, carrying out wet condensation and coarse dehydration on an aromatic vinyl monomer-conjugated diene segmented copolymer from solution polymerization to obtain aqueous copolymer particles;
s2, extruding and dehydrating the water-containing copolymer particles to obtain a preform;
and S3, drying the preform by vacuum infrared drying to obtain the aromatic vinyl monomer-conjugated diene segmented copolymer.
11. An aromatic vinyl monomer-conjugated diene block copolymer obtained by drying by the method according to any one of claims 1 to 10.
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