CN105733156A - Preparation method of xanthan gum-lignin powder chloroprene rubber - Google Patents
Preparation method of xanthan gum-lignin powder chloroprene rubber Download PDFInfo
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- CN105733156A CN105733156A CN201410766899.8A CN201410766899A CN105733156A CN 105733156 A CN105733156 A CN 105733156A CN 201410766899 A CN201410766899 A CN 201410766899A CN 105733156 A CN105733156 A CN 105733156A
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- preparation
- lignin
- xanthan gum
- latex
- mass parts
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- 238000002360 preparation method Methods 0.000 title claims abstract description 53
- 239000000843 powder Substances 0.000 title claims abstract description 47
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 54
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
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- 229910001414 potassium ion Inorganic materials 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a preparation method of xanthan gum-lignin modified powdery chloroprene rubber, which comprises the following steps: 1) preparation of the graft latex: sequentially adding neoprene latex, water, xanthan gum, montmorillonite and a molecular weight regulator into a polymerization kettle, replacing with nitrogen, stirring and heating, adding an initiator accounting for 20-30% of the total mass of the initiator when the temperature of the polymerization kettle reaches 20-35 ℃, stirring and heating for 1-3 hours, adding the rest initiator, carrying out graft polymerization reaction at 30-50 ℃, and adding a terminator when the polymerization conversion rate reaches 65-75% to prepare graft latex; 2) agglomeration into powder: adding the grafted neoprene latex into a coagulation kettle, adding lignin at a coagulation temperature of 10-30 ℃, uniformly stirring, adding an isolating agent, and stirring for 20-40 min; adding a coagulant, fully stirring and uniformly mixing, heating to 20-60 ℃, curing for 4-6 hours, and then separating, dehydrating and drying to obtain the modified powdery chloroprene rubber.
Description
Technical field
The invention belongs to the preparation of powdered polychloroprene rubber, relate to adhesive field, especially relate to a class xanthan gum-lignin modification powdered polychloroprene rubber and preparation method thereof.
Background technology
Neoprene is the rubber adhesive of excellent performance, has the premium properties such as high-adhesive-strength, water-fast, oil resistant, antiacid alkali and anticorrosion because of it and is widely used in the industries such as shoe industry, building industry and auto manufacturing.In recent years, along with the development of domestic construction decoration trade, to the quality of adhesive it is also proposed that requirement higher, that update.Due to the impact of Recipe itself or construction environment, glue in use there will be such or such exception.Such as: tack retention hour is not long, it is easy to dead glue；Glue application is poor；The adhesive force of the viscous material (such as PLASTIC LAMINATED, aluminium-plastic panel) of difficulty is strong not；Especially in the winter time, bonding force is remarkably decreased etc..When powdered polychloroprene rubber is used as adhesive, it is possible to be made directly dissolving, saves production cost, reach the purpose saved energy and reduce the cost.
Xanthan gum, is commonly called as Semen Maydis carbohydrate gum, HANSHENGJIAO, is a kind of saccharide, via the complex polysaccharide that the fermentation of sarson Huang sporangium produces, generally via corn starch manufacture.Xanthan gum is repeated to constitute by pentasaccharides unit, and main chain is identical with cellulose, is namely made up of the glucose being connected with β-Isosorbide-5-Nitrae glycosidic bond, and three connected monosaccharide form its side chain: mannose → glucose → mannose.The mannose being connected with main chain is generally modified by acetyl group, and the mannose of side chain terminal and acetone acid generation aldolisation are thus being modified, and the glucose of centre is then oxidized to glucuronic acid.Xanthan gum, except gathering around well-regulated primary structure, also has secondary structure, through X-ray diffraction and determination of electron microscopy, leans on the helical structure of hydrogen bond action and formation rule between xanthan molecules.Relying on faint active force to form netted stereochemical structure between double-spiral structure, this is the tertiary structure of xanthan gum, and it exists with mesomorph form in aqueous.Xanthan gum is white or lurid powder, has excellent thickening property, suspension, emulsibility and a water solublity, and has good heat, ph stability.
Natural lignin is the aromatic polymer compound that a class has three-D space structure, is made up of phenyl-propane, containing phenolic hydroxyl group, methoxyl group and 2, 2-Oxydiphenol key, it is possible to make the reinforcing agent of rubber as white carbon black.Owing to the molecular structure of lignin also existing aromatic radical, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbon back conjugated double bond isoreactivity group, therefore can carry out aoxidizing, reduce, be hydrolyzed, alcoholysis, acidolysis methoxyl group, Suo Ji, photodissociation, phthalein, many chemical reactions such as sulfonation, alkylation, halogenation, nitrated, polycondensation or graft copolymerization.Wherein, particularly important effect can be shown in the application of research lignin with oxidation, phthalein, sulfonation, polycondensation and graft copolymerization isoreactivity again, also be the important channel expanding its application simultaneously.Industrial lignin is mainly derived from the waste water from cooking of paper-making pulping industry, and the whole world can produce 30,000,000 tons every year, but utilization rate is not high.Current China only has the industrial lignin (mainly lignosulphonates) of 6% to be utilized, all the other major parts make waste discharge, severe contamination rivers.
Montmorillonite main component montmorillonite, is that layer is contained within cation and is mainly sodium ion, magnesium ion, calcium ion, and next has potassium ion, lithium ion etc. by two-layer Si-O tetrahedron and one layer of Al-O octahedron, the phyllosilicate crystal of composition.Research in recent years shows: rubber/montmorillonite nanocomposites has the high intensity of excellence, high rigidity, a performance such as high fire-retardance, and montmorillonite wide material sources are cheap, receive more and more attention.
CN201210232822.3 industrial lignin reinforced rubber and preparation method thereof, is characterized in that: by lignin dispersion and the coprecipitated solidification of latex.CN200810027887.8 industrial lignin strengthens the coblended elastomer material filled, it is made up of elastomers such as lignin and rubber, plastics or rubber-plastic composites, blended employing high-voltage high-speed high-temperature mixing method, make the modified condensation of lignin and the boundary of the mixing of elastomer, lignin and elastomer process and combine, once complete.CN201110413962.6 gutta percha and the preparation method of lignin composite material, heat 65-100 DEG C of softening caking by thick glue；By thick for the Cortex Eucommiae containing lignin glue with coupling agent modified, after plasticating mixing with compounding ingredient uniformly, then sulfidization molding.CN89109494.6 mono-kind utilizes lignin as the method for rubber reinforcing filler, it is characterised in that first prepare lignin formaldehyde resin；Again by mixing uniformly to nitrile rubber and lignin formaldehyde resin in mixing process.The preparation method of a CN03113395.9 high-boiling alcohol lignin rubber modified additive, the steps include: to carry out rubber to plasticate after a period of time, add sulfur or other vulcanizing agents, metal-oxide, the auxiliary agents such as stearic acid are mixing, then are separately added into the derivant of high-boiling alcohol lignin and high-boiling alcohol lignin, white carbon black, adding accelerator and age resistor after reclaiming by plastification a period of time, after refining cementing bundle, at room temperature ripening vulcanizes after 24 hours under proper condition.CN200910043022.5 lignin-modified kaolin and the application as rubber reinforcing filler thereof, in 100 parts of rubbers, add the lignin-modified kaolin 1～100 part after dehydration, mixing 2～4h in mill, make rubber master batch, make lignin-modified kaolin/rubber composite according still further to existing method.
The preparation method of a CN200810123428.X graft modification protein-based adhesive, belongs to field of adhesive technology.The present invention adopts redox system initiator, reacts a period of time at a certain temperature, connects vinyl monomer side chain, it is thus achieved that graft modification protein-based adhesive on protein backbone.Described thickening agent is xanthan gum, sodium alginate, hydroxypropyl starch ether, propylene glycol alginate, gelatin, cyclodextrin, pectin, carrageenan, agar, sesbania gum etc..CN99802589.5 the present invention relates to a kind of from rubber and/or elastomer to its method being prepared, have embedding assorted particulate water-absorbent material therein and crosslinking and processing aid and modifying agent concurrently containing rubber/elastomer component matrix.Absorptive substance is the assembly of (A) polysaccharide and (B) high-hydroscopicity synthetic polymer, and wherein (A) polysaccharide is selected from the starch derivatives beyond cellulose, starch, graft type starch, amylose, amylopectin, glucosan, pectin, inulin, chitin, xanthan gum, alginic acid etc..CN201210442657.4 environment-friendly type building adhesive, comprises xanthan gum composition.The preparation method of a CN200910071462.1 aqueous polymer composite adhesive, preparation method includes preparing performed polymer；Prepare mixed solution；Being joined by performed polymer in mixed solution, isocyanate emulsion is prepared in stirring；Isocyanate emulsion is mixed with aqueous high molecular, stirs and namely obtain aqueous polymer composite adhesive.By polyvinyl alcohol, polyacrylamide, acrylic acid, methacrylate polymer, Polyethylene Glycol, polyethylene glycol oxide, poly, polyvinylpyrrolidone, starch, cellulose ether, chitin, xanthan gum etc., one or more form aqueous high molecular.CN200610114100.2 adhesive without formaldehyde and preparation method thereof, one of which component includes polyvinyl alcohol, xanthan gum, modified starch, vegetable protein powder, glutamic acid etc..The preparation method of CN201210133063.5 phenolic resin adhesive modified lignin resin and starch composite material, method is: 1) by lignin: starch: phenol adds catalyst reaction by proportioning 1:0.3～0.6:2～4 when about fixed temperature；2), after being synthesized, finished product is obtained.The biomass-based Phenolic resin wood adhesive preparation method of CN201210136647.8 mono-kind, wherein comprising lignin is raw material.
The preparation method of a CN200910013774.7 oil-extended montmorillonite-extended solution co-coagulating rubber, joins in rubber solutions by organic modification montmonrillonite, oil, coupling agent, age resistor, stirs 1-30 minute；Above-mentioned solution passes into steam, utilizes separated device, solvent naphtha is steamed and reclaims；Drying prepares oil-extended montmorillonite-extended solution co-coagulating rubber.The preparation method of a CN200910013773.2 oil-extended montmorillonite-extended latex coprecipitation rubber, joins in rubber latex by organic modification montmonrillonite or unmodified montmorillonite suspension liquid, coupling agent and age resistor, and temperature keeps 30-80 DEG C to stir 1-30 minute；Said mixture adds oil emulsion and stirs 1-30 minute；Again respectively by said mixture and flocculating agent, Bronsted acid synchronizes and is gradually added in inorganic salt and flocculant aqueous solution to stir 1-30 minute, keeps pH at 3-4；Adding inorganic base adjustment pH value is 7, flocculates while stirring, and flocculate, through dehydration, dries and prepares oil-extended montmorillonite-extended latex coprecipitation rubber.
US2010300488 (A1) describes a kind of adhesive and contains thickening agent xanthan gum.US4210475A describes a kind of rubber compound, contains rubber ethylene yl pyridines/styrene/butadiene copolymers and the product of a small amount of lignin amine resorcinol-formaldehyde.US4477612A describes a kind of method using lignin reinforcing rubber in mixing process.US2538809 (A) describes the polymer of a kind of elastomeric material, can contain lignin in the filler of reinforcement.US3167523 (A) describe lignin strengthen rubber, heat modification lignin then with rubber co-precipitation.What US3296158 (A) described the mixture of a kind of lignin and the naturally occurring or synthetic rubber of latex reaches co-precipitation by adding multivalent metal salt, and multivalent metal salt is aluminum, magnesium calcium and zinc salt.
US2007054121, US2008248308 (A1) describe a kind of cold coating, and this resin can include the water-soluble polymer of film, such as starch, carboxymethyl cellulose, hydroxyethyl cellulose, and xanthan gum.JP2004352892 describes a kind of mechanical stability for improving nature rubber latex, can add polyvinyl alcohol and xanthan gum mixtures.EP2104710 (A1), GB2370574 describe in a kind of tire composition containing xanthan gum.
Both domestic and external being reported as improves natural rubber or elastomeric performance, and adds lignin or direct and latex mechanical blending in the course of processing, also has the report containing xanthan gum in tire composition.
Summary of the invention
It is an object of the invention to provide a kind of directly cohesion a kind of modified powder neoprene of pulverizing technology preparation by xanthan gum with polychloroprene latex grafting.Adopt the powdered polychloroprene rubber prepared by this method, due to xanthan gum and polychloroprene latex generation grafting, improve the neoprene bonding force as adhesive, as peel strength is higher；The montmorillonite added can improve the combination property of neoprene, and owing to can add lignin in coacervation process, lignin interacts with montmorillonite, adds the compatibility of montmorillonite and neoprene, play strengthening action, better improve the mechanical property of neoprene.The method of modifying of this powdered polychloroprene rubber is simple to operate, product stable storing, and range of application is more extensive.
The preparation method of powdered polychloroprene rubber of the present invention, concrete steps include:
1) preparation of graft latex: (grafting xanthan gum, montmorillonite) is sequentially added into polychloroprene latex, water, xanthan gum, montmorillonite, molecular weight regulator in polymeric kettle, after replacing with nitrogen, stirring, heating, the initiator accounting for initiator gross mass 20%～30% is added when still temperature to be polymerized reaches 20～35 DEG C, agitating heating 1～3 hour, add residue initiator, graft polymerization reaction is carried out at 30～50 DEG C, when polymerisation conversion reaches 65%～75%, add terminator, prepare graft latex；
2) condensation powdering: (addition lignin) takes grafted CR adhesive breast and add condensing field, under 10～30 DEG C of condensation temperatures, adds lignin, is stirring evenly and then adding into interleaving agent, stir 20～40min；Add flocculating agent, be sufficiently stirred for mix homogeneously, be warmed up to 20～60 DEG C of ripenings 4～6 hours, then separated, dehydration, dry prepare modified powder neoprene.
Being added at twice by initiator in the present invention, the initiator that first time adds makes lignin and polychloroprene latex priming reaction, forms mother solution, and second time adds initiator so that continue reaction, forms grafted copolymerized emulsion.Initiator adds at twice, it is possible to make reaction more steadily, more complete.
" part " of being not specifically noted in the present invention each means mass parts.Middle-molecular-weihydroxyethyl regulator of the present invention, initiator, terminator addition all with polychloroprene latex 100 mass parts for benchmark.
Molecular weight regulator of the present invention, initiator, terminator are auxiliary agent generally in the art, all can adopt kind commonly used in the art；Its addition is also well known to a person skilled in the art the conventional amount used required according to latex grafting reaction, and the reagent namely reaching industrial goods grade all can adopt in the present invention.
In order to ensure higher percent grafting, adding 50～160 parts of water in the polychloroprene latex that 100 parts of solid contents are 25%～35%, the mass concentration controlling graft latex is 20%～30%.
With polychloroprene latex 100 mass parts for benchmark, in the present invention, xanthan gum consumption (pure material) is 1～4 part, it is preferable that 3～4 parts.
In the present invention, xanthan gum adds as a solution in the course of the polymerization process, the preparation process of solution is: with polychloroprene latex 100 mass parts for benchmark, in agitator, adds 50～400 mass parts water, 1～4 part of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum.
With polychloroprene latex 100 mass parts for benchmark, in the present invention, montmorillonite consumption (pure material) is 1～5 part, it is preferable that 1～3 part.
In the present invention, montmorillonite preferably adds in the preparation system of graft latex in form of slurry, the preparation process of serosity is: with polychloroprene latex 100 mass parts for benchmark, in agitator, adds 10～50 mass parts water, 1～5 part of montmorillonite, starts agitator stirring and is uniformly dispersed to montmorillonite.
Middle-molecular-weihydroxyethyl regulator of the present invention is sulfur or regulator fourth, and consumption is 0.2～1.4 part, it is preferable that 0.6～1.0 part.
In the present invention, initiator both can use water-soluble inorganic peroxide heat decomposition type initiator, it is used as the oxidation-reduction initiator being made up of water-soluble inorganic peroxide and reducing agent, for the powder-product that prepared crystal property is good, the oxidation-reduction initiator (mol ratio 1:1) being preferably made up of water-soluble inorganic peroxide and reducing agent, such as potassium peroxydisulfate-sodium sulfite；Consumption is 0.2～1.0 part.
In the present invention, graft latex polymerization temperature is 30～50 DEG C, it is preferable that 40～50 DEG C.
In the present invention, glycerol polymerization conversion rate control is 65%～75%, for reducing gel content, it is preferable that 65%～70%.
In the present invention, phthalic acid dibutyl ester selected by terminator, and consumption is 2～10 parts.
With polychloroprene latex 100 mass parts for benchmark, in coacervation process of the present invention, lignin consumption (pure material) is 0.2～1 part, it is preferable that 0.4～0.6 part.
In the present invention, lignin preferably adds in graft latex coacervation process as a solution, the preparation process of solution is: with polychloroprene latex 100 mass parts for benchmark, in agitator, adds 5～10 mass parts water, 0.2～1 part of lignin, starts agitator stirring and is completely dissolved to lignin.
In the present invention, soaps selected by interleaving agent, it is preferable that isproportionated potassium rosinate, consumption is 4～16 parts, it is preferable that 5～10 parts.
In the present invention, flocculant is the inorganic acids such as hydrochloric acid, sulphuric acid, it is preferable that hydrochloric acid, and consumption is 2～10 parts, it is preferable that 3～6 parts.
In the present invention, mineral acid sodium salt selected by flocculating agent, and such as sodium sulfate, sodium chloride etc., it is preferable that sodium chloride, mass concentration is 15%～20%, and every 100 parts of graft latex consumptions are 4～20 parts, it is preferable that 5～10 parts.
In the present invention, after cohesion, powder particle curing temperature is 20～60 DEG C, it is preferable that 40～50 DEG C, 4～6 hours curing times.
The preparation method that present invention also offers a kind of preferred a kind of xanthan gum-lignin modification powdered polychloroprene rubber, concrete steps include:
1) preparation of graft latex: (grafting xanthan gum, montmorillonite) with polychloroprene latex for 100 mass parts meters, being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 50～160 parts of water, 1～4 part of xanthan gum, 1～5 part of montmorillonite, 0.2～1.4 part of molecular weight regulator, after replacing with nitrogen, stirring, heating, the initiator accounting for initiator gross mass (0.2～1.0 part) 20%～30% is added when still temperature to be polymerized reaches 20～35 DEG C, agitating heating 1～3 hour, add residue initiator, graft polymerization reaction is carried out at 30～50 DEG C, when polymerisation conversion reaches 65%～75%, add 2～10 parts of terminators, prepare graft latex；
2) condensation powdering: (addition lignin) takes 100 parts of grafted CR adhesive breasts and add condensing field, under 10～30 DEG C of condensation temperatures, adds 0.2～1 part of lignin, is stirring evenly and then adding into 4～16 portions of interleaving agents, stirs 20～40min；Add 4～16 parts of flocculating agents, be sufficiently stirred for mix homogeneously, be warmed up to 20～60 DEG C of ripenings 4～6 hours, then separated, dehydration, dry prepare modified powder neoprene.
Xanthan gum is to be sent out liquor-saturated by saccharide through Xanthomonas campestris, the outer many pools of microorganism of the born of the same parents of generation.Xanthan molecules is made up of D glucose, D mannose, D glucuronic acid, acetyl group and acetone acid, and relative molecular mass is 2 × 106～5 × 107Between, the side chain of the glucityl main chain that its primary structure is connected by β (1 → 4) key and trisaccharide unit forms；Its side switch is alternately formed by connecting by D mannose and D glucuronic acid, and molecular ratios is 2:1；Trisaccharide side chain is connected with main chain with α (1 → 3) chain with the D mannose of acetyl group by C6 position; with the form of acetal with acetone acid on the D mannose residue of side chain terminal, its higher structure is to be maintained formation spiral and multi-spiral between side chain and main chain by hydrogen bond.Its secondary structure be side chain around main chain backbone reverse-winding, by hydrogen bond maintain formation bar-shaped double-spiral structure.The tertiary structure of xanthan gum is bar-like double-spiral structure and asks the spiral complex combining formation by faint non-covalent bond.Xanthan gum colloidal sol molecule can form the spiral copolymer of superjunction crossed belt shape, constitutes the network structure of fragile similar glue, has very strong stable emulsifying effect.It being added in the course of the polymerization process, xanthan gum with polychloroprene latex generation graft reaction, can form network structure, and the fabulous combination property improving polymer, such as peel strength.
Montmorillonite is the silicate of layer structure, namely it is aluminum or magnesian octahedron by central core, the outer layer structure constituted by silicon dioxide tetrahedron of layer is formed, this tetrahedron and octahedral close-packed structure make it have the lattice arrangement of high-sequential, its reinforcement mechanism is owing to specific surface area and the area/thickness of montmorillonite crystal layer are bigger than all, gas can be effectively hindered to divide all bigger, gas can be effectively hindered to divide all bigger, can effectively hinder gas molecule diffusion in sizing material, its motion path is made to be greatly prolonged, high molecular warm-up movement simultaneously is subject to the restriction of montmorillonite layer, slow down gas diffusion in rubber and infiltration, nano composite material is made to have high air-tightness.
Lignin is a kind of polyhydroxy meshing compound of amorphism macromolecule containing hindered phenol structure, contain various active functional group simultaneously, such as hydroxyl, carbonyl, carboxyl, methyl and side-chain structure, wherein hydroxyl exists more in lignin, exists with alcoholic extract hydroxyl group and two kinds of forms of phenolic hydroxyl group.In lignin, the hydroxyl of rich content can form hydrogen bond with the pi-electron cloud of the conjugated double bond of neoprene, thus playing the effect of reinforced rubber.Lignin also acts as the effect of flocculant in the reaction so that becomes powder to be more uniformly distributed, condenses more thorough.
The principle of xanthan gum and polychloroprene latex grafting is in that, initiator persulfate S2O8 2-→2SO4 2-, 2SO4 2-+H2O→HSO4 -+HO-, SO4 2-And HO-The hydrogen on xanthan molecules can be captured, make xanthan gum slough a hydrogen atom and form xanthan gum free radical (XG), with polychloroprene latex generation graft reaction；Initiator adds at twice, makes reaction more steady, it is to avoid occur sudden and violent poly-；The addition of montmorillonite, plays the effect of In-sltu reinforcement, owing to its bigger physics makes polychloroprene latex be more easy to into powder with chemisorption；In lignin, the hydroxyl of rich content can form hydrogen bond with the pi-electron cloud of the conjugated double bond of rubber, thus playing the effect of reinforced rubber；Lignin can interact with montmorillonite, improves the compatibility of montmorillonite and rubber, plays better strengthening action；Between hydroxyl and the neoprene of lignin molecule, strong interaction is also beneficial to improve its crosslink density, improves the mechanical property of neoprene.
Modified powder neoprene prepared by the present invention has the feature that powder diameter 0.40mm～1.50mm, powder formation rate >=99.5%, ash≤0.10%, fugitive constituent≤0.10%, swelling time tens of second, dissolution time 2～4 hours, peel strength >=90N/cm.
Detailed description of the invention
Below by specific embodiment, the preparation method of the modified powder neoprene of the present invention is described in further detail.
Polychloroprene latex: domestic polychloroprene latex CR244, total solid substance is 30～40%.Other reagent are commercially available industrial goods.
Xanthan gum: the industry of Henan perseverance Thailand, food additive specification.
Lignin: Shouguang Yu Jiang Bioisystech Co., Ltd, index: palm fibre (Huang) brown powder, water-insoluble≤1.5%, pH value 8～10, moisture content≤5.0%, fineness 80 order percent of pass >=95%.
Montmorillonite: Zhejiang Fenghong New Material Co., Ltd., model DK, nanoscale.
Experimental facilities: Muffle furnace, water-bath constant temperature oscillator, peel strength tester OM-898 type, FM11 type high temperature furnace, electronic balance AE100.
Method of testing: mean diameter, adopted sieve method, sieves 12,16,20,28 orders with Tyler and divides 4 screenings to measure, particle size range 0.5～1.0mm.
Powder formation rate, adopts mass method to measure, and weighs with the HangpingJA2003 type balance that Shanghai balance equipment factory produces.
Peel strength, the OM-898 type peel strength tester adopting Dongguan City Oran detection equipment company limited to produce, measure according to Q/HS25 2007.
Ash, GB/T4498-1997；Fugitive constituent, GB/T24131-2009.
Embodiment 1
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 50 mass parts water, 1 part of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In another agitator, add 10 mass parts water, 1 part of montmorillonite, start agitator stirring and be uniformly dispersed to montmorillonite；In another agitator, add 10 mass parts water, 0.2 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 50 parts of water, 1. middle xanthan gum and montmorillonite, 0.2 part of regulator fourth, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 20 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.04 part (the 20% of 0.2 part) potassium peroxydisulfate-sodium sulfite acid, agitating heating 3 hours, add 0.16 part of potassium peroxydisulfate of residue-sodium sulfite acid, graft polymerization reaction is carried out at 30 DEG C, when polymerisation conversion reaches 65%, add 2 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 10 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 4 parts of isproportionated potassium rosinate, stir 20min；Add 4 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 20 DEG C of ripenings 4 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.40mm～1.50mm, powder formation rate 99.8%, ash 0.8%, fugitive constituent 0.10%, swelling time tens of second, dissolution time 3 hours, peel strength 92N/cm.
Comparative example 1
Experimentation is with embodiment 1, and simply the preparation of graft latex does not add xanthan gum.Experimental result is: powder diameter 0.20mm～1.80mm, powder formation rate 95.0%, ash 0.18%, fugitive constituent 0.15%, swelling time hundreds of second, dissolution time 8 hours, peel strength 85N/cm.
Embodiment 2
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 100 mass parts water, 1 part of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In another agitator, add 20 mass parts water, 1 part of montmorillonite, start agitator stirring and be uniformly dispersed to montmorillonite；In another agitator, add 5 mass parts water, 0.2 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 100 parts of water, 1. middle xanthan gum and montmorillonite, 1.4 parts of regulator fourths, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 30 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.06 part (the 20% of 0.3 part) potassium peroxydisulfate-sodium sulfite acid, agitating heating 3 hours, add residue potassium peroxydisulfate-sodium sulfite acid 0.24 part, graft polymerization reaction is carried out at 30 DEG C, when polymerisation conversion reaches 75%, add 10 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 30 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 10 parts of isproportionated potassium rosinate, stir 40min；Add 4 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 40 DEG C of ripenings 5 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.50mm～1.50mm, powder formation rate 99.9%, ash 0.10%, fugitive constituent 0.9%, swelling time tens of second, dissolution time 4 hours, peel strength 94N/cm.
Comparative example 2
Experimentation is with embodiment 2, and simply the preparation of graft latex does not add montmorillonite.Experimental result is: powder diameter 0.50mm～2.0mm, powder formation rate 92.6%, ash 0.15%, fugitive constituent 0.19%, swelling time number every minute and second, dissolution time 7 hours, peel strength 88N/cm.
Embodiment 3
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 300 mass parts water, 4 parts of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In another agitator, add 30 mass parts water, 5 parts of montmorillonites, start agitator stirring and be uniformly dispersed to montmorillonite.In another agitator, add 10 mass parts water, 1 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 160 parts of water, 1. middle xanthan gum and montmorillonite, 1.0 parts of regulator fourths, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 35 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.1 part (the 20% of 0.5 part) potassium peroxydisulfate-sodium sulfite acid, agitating heating 2 hours, add residue potassium peroxydisulfate-sodium sulfite acid 0.4 part, graft polymerization reaction is carried out at 50 DEG C, when polymerisation conversion reaches 70%, add 5 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 20 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 16 parts of isproportionated potassium rosinate, stir 40min；Add 10 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 60 DEG C of ripenings 4 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.50mm～1.20mm, powder formation rate 99.5%, ash 0.10%, fugitive constituent 0.08%, swelling time tens of second, dissolution time 2 hours, peel strength 90N/cm.
Comparative example 3
Experimentation is with embodiment 3, and simply the preparation of graft latex does not add xanthan gum, montmorillonite.Experimental result is: powder diameter 0.30mm～1.50mm, powder formation rate 94.8%, ash 0.15%, fugitive constituent 0.16%, swelling time hundreds of second, dissolution time 5 hours, peel strength 81N/cm.
Embodiment 4
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 400 mass parts water, 1 part of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In agitator, add 40 mass parts water, 1 part of montmorillonite, start agitator stirring and be uniformly dispersed to montmorillonite；In another agitator, add 5 mass parts water, 1 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 50 parts of water, 1. middle xanthan gum and montmorillonite, 0.5 part of regulator fourth, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 25 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.3 part (the 30% of 1.0 parts) potassium peroxydisulfate-sodium sulfite acid, agitating heating 3 hours, add residue potassium peroxydisulfate-sodium sulfite acid 0.7 part, graft polymerization reaction is carried out at 30 DEG C, when polymerisation conversion reaches 65%, add 10 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 15 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 5 parts of isproportionated potassium rosinate, stir 30min；Add 5 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 40 DEG C of ripenings 4 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.40mm～1.50mm, powder formation rate 99.8%, ash 0.08%, fugitive constituent 0.10%, swelling time tens of second, dissolution time 3 hours, peel strength 95N/cm.
Comparative example 4
Experimentation, with embodiment 4, does not simply add lignin in cohesion.Experimental result is: powder diameter 0.20mm～2.50mm, powder formation rate 90.3%, ash 0.18%, fugitive constituent 0.15%, swelling time hundreds of second, dissolution time 8 hours, peel strength 87N/cm.
Embodiment 5
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 50 mass parts water, 2 parts of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In another agitator, add 30 mass parts water ,～5 parts of montmorillonites, start agitator stirring and be uniformly dispersed to montmorillonite；In another agitator, add 10 mass parts water, 1 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 100 parts of water, 1. middle xanthan gum and montmorillonite, 0.8 part of regulator fourth, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 30 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.2 part (the 20% of 1.0 parts) potassium peroxydisulfate-sodium sulfite acid, agitating heating 2 hours, add residue potassium peroxydisulfate-sodium sulfite acid 0.8 part, graft polymerization reaction is carried out at 30 DEG C, when polymerisation conversion reaches 70%, add 5 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 10 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 10 parts of isproportionated potassium rosinate, stir 40min；Add 10 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 20 DEG C of ripenings 5 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.50mm～1.50mm, powder formation rate 99.5%, ash 0.10%, fugitive constituent 0.10%, swelling time tens of second, dissolution time 4 hours, peel strength 90N/cm.
Comparative example 5
Experimentation is with embodiment 5, and simply the preparation of graft latex does not add xanthan gum, does not add lignin in cohesion.Experimental result is: powder diameter 0.30mm～2.0mm, powder formation rate 90.5%, ash 0.16%, fugitive constituent 0.20%, swelling time hundreds of second, dissolution time 6 hours, peel strength 83N/cm.
Embodiment 6
1. the dispersion of xanthan gum, montmorillonite and lignin: in agitator, adds 100 mass parts water, 2 parts of xanthan gum, starts agitator stirring and is completely dissolved to xanthan gum；In another agitator, add 20 mass parts water, 3 parts of montmorillonites, start agitator stirring and be uniformly dispersed to montmorillonite；In another agitator, add 5 mass parts water, 0.2 part of lignin, start agitator stirring and be completely dissolved to lignin.2. the preparation of graft latex: being sequentially added into 100 parts of solid contents in polymeric kettle is the polychloroprene latex of 25%～35%, 120 parts of water, 1. middle xanthan gum and montmorillonite, 0.6 part of regulator fourth, after replacing with nitrogen, stirring, heating, add when still temperature to be polymerized reaches 30 DEG C and account for potassium peroxydisulfate-sodium sulfite acid gross mass 0.24 part (the 30% of 0.8 part) potassium peroxydisulfate-sodium sulfite acid, agitating heating 2 hours, add residue potassium peroxydisulfate-sodium sulfite acid 0.56 part, graft polymerization reaction is carried out at 50 DEG C, when polymerisation conversion reaches 75%, add 6 parts of phthalic acid dibutyl esters, prepare graft latex；3. condensation powdering: take 100 parts of grafted CR adhesive breasts and add condensing field, under 25 DEG C of condensation temperatures, adds lignin in 1., is stirring evenly and then adding into 8 parts of isproportionated potassium rosinate, stir 30min；Add 10 parts of hydrochloric acid, be sufficiently stirred for mix homogeneously, be warmed up to 50 DEG C of ripenings 5 hours, then separated, dehydration, dry prepare modified powder neoprene.Experimental result is: powder diameter 0.40mm～1.50mm, powder formation rate 99.8%, ash 0.10%, fugitive constituent 0.09%, swelling time tens of second, dissolution time 2 hours, peel strength 91N/cm.
Comparative example 6
Experimentation is with embodiment 6, and simply the preparation of graft latex does not add montmorillonite, does not add lignin in cohesion.Experimental result is: powder diameter 0.20mm～1.50mm, powder formation rate 90.1%, ash 0.17%, fugitive constituent 0.15%, swelling time hundreds of second, dissolution time 5 hours, peel strength 82N/cm.
Claims (10)
1. a preparation method for xanthan gum-lignin powdered polychloroprene rubber, concrete steps include:
1) preparation of graft latex: be sequentially added into polychloroprene latex, water, xanthan gum, montmorillonite and molecular weight regulator in polymeric kettle, after replacing with nitrogen, stirring, heating, add the initiator accounting for initiator gross mass 20%～30%, agitating heating 1～3 hour when still temperature to be polymerized reaches 20～35 DEG C, add residue initiator, graft polymerization reaction is carried out at 30～50 DEG C, when polymerisation conversion reaches 65%～75%, add terminator, prepare graft latex；
2) condensation powdering: take grafted CR adhesive breast and add condensing field, under 10～30 DEG C of condensation temperatures, adds lignin, is stirring evenly and then adding into interleaving agent, stir 20～40min；Add flocculating agent, be sufficiently stirred for mix homogeneously, be warmed up to 20～60 DEG C of ripenings 4～6 hours, then separated, dehydration, dry prepare modified powder neoprene.
2. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described xanthan gum is 1～4 part.
3. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described xanthan gum is 3～4 parts.
4. preparation method as claimed in claim 1, it is characterized in that described xanthan gum adds as a solution in the course of the polymerization process, the preparation process of solution is: with polychloroprene latex 100 mass parts for benchmark, adds 50～400 mass parts water, 1～4 part of xanthan gum, stirring to xanthan gum is completely dissolved.
5. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described montmorillonite is 1～5 part.
6. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described montmorillonite is 1～3 part.
7. preparation method as claimed in claim 1, it is characterized in that in the preparation system that described montmorillonite adds graft latex in form of slurry, the preparation process of serosity is: with polychloroprene latex 100 mass parts for benchmark, add 10～50 mass parts water, 1～5 part of montmorillonite, stirring to montmorillonite is uniformly dispersed.
8. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described lignin is 0.2～1 part.
9. preparation method as claimed in claim 1, it is characterised in that with polychloroprene latex 100 mass parts for benchmark, the addition of described lignin is 0.4～0.6 part.
10. preparation method as claimed in claim 1, it is characterized in that described lignin adds in graft latex coacervation process as a solution, the preparation process of solution is: with polychloroprene latex 100 mass parts for benchmark, add 5～10 mass parts water, 0.2～1 part of lignin, stirring to lignin is completely dissolved.
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Application publication date: 20160706 |