CN101481459A - Micropore ligno-cellulose ultramicro powder, as well as preparation method and application thereof - Google Patents
Micropore ligno-cellulose ultramicro powder, as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to microporous lignocelluloses submicron powder, the application method and the application thereof, belonging to the chemical industry field. The method takes materials containing microporous lignocelluloses as raw materials which are physically smashed and ground many times. The modification treatment is carried out on intermediate products by a chemical treatment method among each physical smashing and grinding process so as to obtain the submicron powder with the fineness of larger than 500 mesh and about one micrometer of micropores distributed on the powder. The submicron can serve as an industrial additive to be applied to textile functional coating, synthetic leather, paint, leather products coating, can increase the waterproof, moisture absorption, combining fastness and aging resistant performance of the products, has vapor permeability and extensive use.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of preparation method who can be used as the fine powder of modification lignocellulose of functional additive, and the product that makes with this method is as the application on the industrial additive.
Background technology
Functional additive in the chemical field is very abundant, generally is added in some chemical composition reaching or to promote the property of these chemical compositions, such as, be applied to take in the textile surface coating, can reach or strengthen effects such as saturating wet, waterproof.
200710145401.6 1 kinds of water-proof moisture-permeation coating agent compositions of the previous patent application of applicant and application thereof disclose a kind of water-proof moisture-permeation coating agent composition, add the fine powder of a certain amount of micropore ligno-cellulose in having the coating-forming agent of water-proof function.The fine powder of the micropore ligno-cellulose that adds in the prior art, be to be that xylogen and cellulosic wooden unit or wooden stick's core are crushed to the powder that certain fineness (more than 80 orders) is made with the main body composition, basically be natural material to be carried out physical pulverization handle, on the one hand, for keeping distinctive microvoid structure in the starting material, can not be more further refinement in order to avoid destroy microvoid structure, on the other hand, the excessive adhesion phenomenon of stickiness just appears when being crushed to the 400 order left and right sides, also can't continue refinement, micropore destroys serious.The 3rd, owing to there is not modification to handle, reactive relatively poor, every performance washing fastness is lower, therefore, adds that to combine stability than the coating of volume particle size powder and fabric not good enough, and ageing resistance is poor, is necessary to carry out degree of depth improvement.
Summary of the invention
The objective of the invention is on the basis of original technology, a kind of method for preparing the trickleer micropore ligno-cellulose ultramicro powder of particle diameter is provided.
The preparation method of a kind of micropore ligno-cellulose ultramicro powder of the present invention, with the material that contains micropore ligno-cellulose is raw material, through repeatedly physical pulverization grinding, and between each physical pulverization is ground, adopt chemical treatment method that middle product is carried out modification and handle, obtain fineness greater than 500 purpose super-fine powder.
Wherein, described raw material is for being selected from plants such as softwood, pourous wood, Gramineae, and one or more in preferred big waste of flax core, jute bar core, falx straw core, sisal hemp bar core, ramie stalk core and the bamboo mix use.
The preparation method of this micropore ligno-cellulose ultramicro powder specifically may further comprise the steps:
1) raw material pulverizing: raw material is crushed to the irregular granular meal of 20-80 order with pulverizer;
2) pre-treatment: under 80～160 ℃, with meal heated and stirred 1～6 hour in 2～20g/L caustic soda, 0～10g/L sodium sulfide solution, precipitation is dried to moisture content 0.5～1wt%, obtains the modification meal;
3) thinning processing: the modification meal is finish-ground to 200～400 order fine powders;
4) activation treatment: under 50～100 ℃, fine powder added in the caustic soda soln that concentration is 1～10g/l stirred 1～5 hour, regulating pH value with dilute hydrochloric acid again is 2, precipitates to be washed to neutrality, dry to water ratio at 0.2～1.0wt%, obtain activating fine powder; Powder and solution weight are than being 1:5～1:20.
5) aggregation processing: under 60-130 ℃, will activate fine powder and obtain the polymerization fine powder in 10～60 minutes with vulcabond solution and polyvalent alcohol mixing stirring reaction; Described vulcabond is a kind of among MDI, TDI, HDI, the HMDI, and consumption is 1～20wt%, and polyvalent alcohol is a kind of in ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, the tetrahydrofuran (THF) etc., and consumption is 0.2～2wt%;
6) miniaturization is handled: with polymerization fine powder regrinding, and screening obtains 500-1000 purpose micropowders, promptly obtains finished product.
Under the product needed bleaching situation, step 2) also comprises bleaching process in, step 2) is specially: under 80～160 ℃, with meal heated and stirred 1～6 hour in 2～20g/L caustic soda, 0～10g/L sodium sulfide solution, filter back discharge opeing flushing, add hydrogen peroxide in throw out, 80～100 ℃ were stirred 3～30 hours down; Then, add the acetic acid neutralization, filtering, be washed to precipitation pH value is 5～8; Dry to moisture content 0.5～1wt%, obtain the modification meal.
Among the preparation method of above-mentioned micropore ligno-cellulose ultramicro powder, step 1) adopts jaw crusher, cone crusher, roller crusher or impact crusher to pulverize; Step 3) adopts Raymond mill, ultra-fine mill or ball mill grinding; Step 6) adopts vibromill or high pressure micro ball-mill correct grinding, adopts gas delivery to filter out super-fine powder.
Another purpose of the present invention is to provide the fineness that is prepared by this method at 500～1000 purpose micropore ligno-cellulose ultramicro powders.Especially, wherein 600～800 order powders are more than 70%.
Especially, has micropore on the described ultrafine powder.
Another object of the present invention is to provide the application of this fine powder as industrial additive, is specially, and can add in the textile coating agent waterproof that improves coating, saturating wet, conjugation and ageing-resistant performance to; Can add to heightens the color in coating, the paint reaches hyperchromic effect; Can add to and improve leather ageing-resistant performance or the like in the leather coating agent.
Compared with the prior art the present invention has following advantage:
1, in the preparation process of micropore ligno-cellulose powder of the present invention, physical treatment and chemical treatment combine, make the powder embrittlement by alkalinisation treatment, by the microvoid structure in the activation treatment expansion powder, powder and polymkeric substance are passed through graft reaction, and, can obtain the inaccessiable effect of simple physical thinning in conjunction with the physics process for refining.
2, the super-fine powder for preparing of the present invention, fineness can reach 500～1000 orders, and can still keep microvoid structure.
3, the coated fabric water pressure resistance height that uses fine powder of the present invention to make wets thoroughly, and coating combines firmly with fabric, and ageing-resistant performance significantly improves; Add in coating, the paint and can heighten the color, reach hyperchromic effect, reduce the consumption of pigment; Add in the leather coating agent and can improve leather ageing-resistant performance or the like.
Description of drawings
Fig. 1 is different treatment stage powder Electronic Speculum figure in the preparation process of the present invention.A is the meal picture, and B is the fine powder picture, and C is the super-fine powder picture.
Embodiment
The mode that the present invention mainly combines by physical treatment and chemical treatment prepares the micropore ligno-cellulose fine powder.Among the present invention, " powder " is general designation, and " super-fine powder " refers in particular to fineness greater than 500 purpose powders.
Among the present invention, employed raw material is the material with natural micropore structure, include but not limited to plants such as softwood, pourous wood, Gramineae, one or more in preferred big waste of flax core, jute bar core, falx straw core, sisal hemp bar core, ramie stalk core and the bamboo mix use; Among the present invention, employed reagent is industrial.
The present invention prepares micropore ligno-cellulose ultramicro powder according to the following steps:
1) raw material pulverizing: above-mentioned raw materials is crushed to the irregular granular powder of 20-80 order (meal) with pulverizer.Used pulverizer can be that jaw crusher (tiger mouth), cone crusher, roller crusher, impact crusher etc. are a kind of.
2) pre-treatment: the lignocellulose meal is put into stainless steel cauldron, add caustic soda, sodium sulphite and water, powder and water ratio are 1:5～1:20, and caustic soda concentration is 2～20g/L, sodium sulphite 0～10g/l.Heated and stirred is handled, 80～160 ℃ of temperature, 1～6 hour time.As the need bleaching, can be after alkaline purification, after the discharge opeing flushing, add hydrogen peroxide, available oxygen concentration 1～10g/l, temperature is 80～100 ℃, the time is 3～30 hours.Then, add the acetic acid neutralization, to be washed to pH value be 6～8.With powder filter, drying, put into the hotblast stove oven dry, 100～140 ℃ of bake out temperatures, control moisture content 0.5～1wt%.This step has mainly removed pectin and xylogen in the meal, and the embrittlement meal is beneficial to following process, obtains the modification meal.
3) thinning processing: will put into correct grinding equipment through pretreated lignocellulose modification meal and grind, and make fine powder, 200 to 400 orders keep its micropore constant.Correct grinding equipment comprises that Raymond mill, ultra-fine mill, ball mill etc. are a kind of, and the time is 2～10 hours, by wind filter control powder granularity.Obtain the lignocellulose fine powder.
4) activation treatment: under 50～100 ℃, fine powder added stir 1～5 hour in the activator solution, regulating pH value with dilute hydrochloric acid again is 2, precipitates to be washed to neutrality, dry to water ratio at 0.2～1.0wt%, obtain activating fine powder; Powder and solution proportion are 1:5～1:20, and described activator is a caustic soda, and working concentration is 1～10g/l, preferred 2g/l～10g/l.
Oven dry: the plain powder of the china-hemp fibers after the activation treatment is filtered, dries, dry through hotblast stove.100～140 ℃ of temperature, the control water ratio is in 0.2～1.0wt%.This step obtains activating fine powder.
5) aggregation processing: lignocellulose is activated fine powder put into reactor, add a certain amount of vulcabond solution, stir certain hour at a certain temperature, add a certain amount of polyvalent alcohol again, mix and stir certain hour.Temperature is 60-130 ℃, and churning time is 10～60 minutes.Vulcabond is a kind of among MDI, TDI, HDI, the HMDI, and consumption is 1～20wt%, and polyvalent alcohol is a kind of in ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, the tetrahydrofuran (THF) etc., and consumption is 0.5～2wt%.This step obtains the polymerization fine powder.
6) miniaturization is handled: will grind through the polymeric fine powder, and obtain micropowders by screening and selection by winnowing, powder is the 500-1000 order.Grinding plant adopts vibromill, high pressure micro ball-mill etc., adopts gas delivery to filter out micro mist, obtains super-fine powder of the present invention.It is multi-functional that this super-fine powder has reactivity, Waterproof Breathable, anti-aging, anti, delustring etc.
The present invention obtains the Performance Detection of super-fine powder:
1, powder microvoid structure observation: the microscopic pattern that uses the different powders of scanning electron microscopic observation, Fig. 1 has shown its microvoid structure, A is raw material meal structure after step 1) is pulverized, and B is a fine powder structure after the step 3) thinning processing, and C handles back super-fine powder structure for the step 6) granular.The photo structure shows, in treating processes of the present invention, kept the microvoid structure of material in the powder all the time, be distributed with the micropore of size about 1um in the finished product super-fine powder, this micropore can see through gas or steam (having vapour permeability), but water droplet can not be seen through.
2, powder fineness is measured: in the preparation process of the present invention, ultramicronising is handled the back powder and is obtained micropowders by screening and selection by winnowing, the powder size is all greater than 500 orders, reach the inaccessiable fineness state of conventional processing (simple physical grinding), film-forming properties, reactivity provide assurance when using for this super-fine powder.
3, reactive mensuration:
The preparation of HAIR COLOR COMPOSITION: add the super-fine powder additive of the present invention of a certain amount of (20wt%) in normal polyurethane coating agent producing process, technology is carried out building-up reactions and is obtained HAIR COLOR COMPOSITION routinely.
The preparation of water-proof coating fabric: fabric through after the waterproofing, calendering, is coated in base cloth with HAIR COLOR COMPOSITION, make have waterproofing and moisture-penetration performances coated fabric as test article.
This coated fabric is carried out correlated performance detect, detected result is referring to table 1.
Table 1:
4, competitive trial: carry out the coating of same base cloth with common PU Waterproof Breathable coating adhesive, make the blank product; Carry out the coating of same base cloth with the common PU glue that adds the common fine powder of 20wt% (200 order), make relatively product, test its water-resistant pressure, vapor transfer rate and aging resistance respectively, compare test the results are shown in Table 2.
Table 2:
*The thermokalite burn-in test is referring to 5 description.
Table 2 experimental data shows, specimen water-proof coating fabric (reference substance and test article) behind the interpolation lignocellulose powder, reducing under the coated weight situation, its compressive strength, the more blank sample of vapor transfer rate are significantly increased, test article is more excellent than the reference substance performance, especially wash 20 times after, its water pressure resistance still can reach 100kpa, illustrate test article coating and fabric to combine stability good, ageing-resistant performance is superior; The increasing of vapor transfer rate shows that the coating of test article can better be had a good sweat.
5, thermokalite burn-in test:
Testing liquid: 10 times of concentration synthetic perspirations require PH in addition〉14,, add glycerine 2g/l;
Test sample: prepare blank sample, reference substance and test article coated fabric with test 3 identical methods.Test method:
1. test: get 5 of every kind of coated fabrics, measure the original water pressure resistance ability of coated fabric, calculating mean value;
2. flood: in the testing liquid with 90 ℃ of each test sample immersions, thorough impregnation 30 minutes.Take out dehydration then.
3. aging oven dry: 70 ℃ were dried by the fire 12 hours in ageing oven.
Test the water pressure resistance ability once more.The test result ginseng is shown in Table 2.Show that the aging ability of test article heat resistanceheat resistant alkali is stronger, the more original water-resistant pressure of water-resistant pressure weakens less, and blank sample and control sample water-resistant pressure then have obviously and weaken.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: the preparation of big waste of flax core super-fine powder
1) raw material pulverizing: big waste of flax core is crushed to 20 order left and right sides meal with jaw crusher.
2) pre-treatment: get the 1kg meal and put into the 50L stainless steel cauldron, add 100g caustic soda, 10g sodium sulphite and water 5L, temperature stirred 6 hours for 80 ℃; To precipitate the powder centrifuge dripping after the filtration, and put into 140 ℃ of hotblast stoves and dry to moisture content 1wt%; Naturally cooling obtains the modification meal.
3) thinning processing: meal is put into Raymond mill grind 2 hours, by wind filter control powder granularity to 200 order fine powders.
4) activation treatment: got 200 order fine powder 1kg and put into the 50L reactor, adding concentration is the caustic soda soln 10kg of 5g/l, and activation treatment was carried out in 50 ℃ of stirrings in 4 hours; The reaction back is about 2 with dilute hydrochloric acid regulator solution to pH value, is washed to neutrality then.Filter, will precipitate the wet-milling drying, through 140 ℃ of hotblast stoves dry to water ratio less than 1.0wt%, obtain activating fine powder.
5) aggregation processing: get activation fine powder 1kg and put into the 50L reactor, add 100gMDI, stir down at 60 ℃, add 5g ethylene glycol again, continue to stir 60 minutes down at 60 ℃, oven dry obtains the polymerization fine powder.
6) miniaturization is handled: with vibromill the polymerization fine powder is ground, obtain greater than 500 micropowders with the screening of gas delivery sieve.
With above-mentioned testing method this routine super-fine powder is detected, powder fineness all more than 500 orders, is distributed with the micropore about 1um on the electron microscopic observation micro mist as a result, make the HAIR COLOR COMPOSITION coated fabric after, apply PU45g/m
2Water pressure resistance 220kpa, wash 20 times after water pressure resistance be 123Kpa, vapor transfer rate 7900g/m
2.24h.
Embodiment 2: the preparation of bleaching big waste of flax core super-fine powder
With embodiment 1 same operation, in step 2) in add bleaching process.Concrete steps 2) be: get the 1kg meal and put into the 50L stainless steel cauldron, add 100g caustic soda, 10g sodium sulphite and water 5L, temperature stirred 6 hours for 80 ℃; Filter back discharge opeing flushing, add the 500mL hydrogen peroxide in throw out, 80～100 ℃ were stirred 3～30 hours down; Then, add the neutralization of an amount of acetic acid, filter, be washed to that to be deposited to pH value be 5～8; To precipitate the powder centrifuge dripping, and put into 140 ℃ of hotblast stoves and dry to moisture content 1wt%; Naturally cooling obtains the modification meal.
By this operation, the meal after can obtaining bleaching.This meal carries out the super-fine powder that obtains after the subsequent disposal, and powder fineness all more than 500 orders, is distributed with the micropore about 1um on the electron microscopic observation micro mist, make the HAIR COLOR COMPOSITION coated fabric after, apply PU45g/m
2Water pressure resistance 213kpa, vapor transfer rate 7950g/m
2.24h, the washing 20 times after water pressure resistance be 102Kpa.Illustrate that the present invention does not influence the proterties of product in conjunction with bleaching process.
Embodiment 3～embodiment 5: the preparation of ligno-cellulose ultramicro powder
Carry out the preparation of multiple lignocellulose according to the operating process of embodiment 1 and the parameter of table 3, and carry out performance test as hereinbefore.
Table 3:
The ligno-cellulose ultramicro powder that the inventive method prepares, powder fineness all more than 500 orders, are distributed with the micropore about 1um on the electron microscopic observation micro mist, make the HAIR COLOR COMPOSITION coated fabric after, apply PU45g/m
2Water pressure resistance more than 200kpa, wash 20 times after water pressure resistance still remain on more than the 100Kpa, associativity is good, has good ageing-resistant performance, also keeps the high ventilation performance simultaneously, vapor transfer rate reaches 5500g/m
2.24h.
Embodiment 6: the application of ligno-cellulose ultramicro powder
One, in the water-proof coating of fabric, uses: in normal polyurethane coating agent producing process, add a certain amount of ligno-cellulose ultramicro powder, carry out building-up reactions as multifunction additive.Usually, addition is 5～90wt% of solid content.
Two, in coating, use: in acrylate or urethane, add the ligno-cellulose ultramicro powder of 5-30wt%, can make coating prevent crack, ageing-resistant, and can reduce the colored pigment consumption.
Three, in leatheroid or wet-process coating, use: in coated material, add the ligno-cellulose ultramicro powder of 10-20wt%, can improve moisture uptake, ageing-resistant, and can reduce cost, strengthen the wood grain sense.
Claims (10)
1, a kind of preparation method of micropore ligno-cellulose ultramicro powder, it is characterized in that, with the material that contains micropore ligno-cellulose is raw material, through repeatedly physical pulverization grinding, and between each physical pulverization is ground, adopt chemical treatment method that middle product is carried out modification and handle, obtain fineness greater than 500 purpose super-fine powder.
2, according to the preparation method of the described micropore ligno-cellulose ultramicro powder of claim 1, it is characterized in that, described raw material is for being selected from plants such as softwood, pourous wood, Gramineae, and one or more in preferred big waste of flax core, jute bar core, falx straw core, sisal hemp bar core, ramie stalk core and the bamboo mix use.
3, according to the preparation method of claim 1 or 2 described micropore ligno-cellulose ultramicro powders, it is characterized in that, specifically may further comprise the steps:
1) raw material pulverizing: raw material is ground into the irregular granular meal of 20-80 order with pulverizer;
2) pre-treatment: under 80～160 ℃, heated and stirred is 1～6 hour in 2～20g/L caustic soda, 0～10g/L sodium sulfide solution, and precipitation is dried to moisture content 0.5～1wt%, obtains the modification meal;
3) thinning processing: the modification meal is finish-ground to 200～400 order fine powders;
4) activation treatment: under 50～100 ℃, fine powder added in the caustic soda soln that concentration is 1～10g/l stirred 1～5 hour, regulating pH value with dilute hydrochloric acid again is 2, precipitates to be washed to neutrality, dry to water ratio at 0.2～1.0wt%, obtain activating fine powder; Powder and solution weight are than being 1:5～1:20;
5) aggregation processing: under 60-130 ℃, will activate fine powder and obtain the polymerization fine powder in 10～60 minutes with vulcabond solution and polyvalent alcohol mixing stirring reaction; Described vulcabond is a kind of among MDI, TDI, HDI, the HMDI, and consumption is 1～20wt%, and polyvalent alcohol is a kind of in ethylene glycol, propylene glycol, butyleneglycol, hexylene glycol, the tetrahydrofuran (THF) etc., and consumption is 0.2～2wt%;
6) miniaturization is handled: with polymerization fine powder regrinding, and screening obtains 500-1000 purpose micropowders, promptly obtains finished product.
4, according to the preparation method of the described micropore ligno-cellulose ultramicro powder of claim 3, it is characterized in that step 2) in also comprise bleaching process, step 2) be specially:
Under 80～160 ℃, with meal heated and stirred 1～6 hour in 2～20g/L caustic soda, 0～10g/L sodium sulfide solution, filter back discharge opeing flushing, add hydrogen peroxide in throw out, 80～100 ℃ were stirred 3～30 hours down; Then, add the acetic acid neutralization, filtering, be washed to precipitation pH value is 5～8; Dry to moisture content 0.5～1wt%, obtain the modification meal.
According to the preparation method of the described micropore ligno-cellulose ultramicro powder of claim 3, it is characterized in that 5, step 1) adopts jaw crusher, cone crusher, roller crusher or impact crusher to pulverize; Step 3) adopts Raymond mill, ultra-fine mill or ball mill grinding; Step 6) adopts vibromill or high pressure micro ball-mill correct grinding, adopts gas delivery to filter out super-fine powder.
6, the micropore ligno-cellulose ultramicro powder for preparing with the arbitrary described method of claim 1 to 5.
7, according to the described micropore ligno-cellulose ultramicro powder of claim 6, it is characterized in that having micropore on the described ultrafine powder.
According to the described micropore ligno-cellulose ultramicro powder of claim 7, it is characterized in that 8, described super-fine powder size-grade distribution is at 500～1000 orders, wherein 600～800 order powders are more than 70%.
9, claim 6 or 7 or 8 described micropore ligno-cellulose ultramicro powders are as the application of industrial functional additive.
According to the described application of claim 9, it is characterized in that 10, micropore ligno-cellulose ultramicro powder is applied in fabric functional coating-forming agent, coating or synthetic leather and the leatheroid coating.
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