CN1312872A - A microparticle system in the paper making process - Google Patents

Abstract

A retention and drainage aid comprising a microparticle system for use in the production of an alkaline and an acid paper product comprises a flocculant polymer and an inorganic particulate material comprising an aluminum substituted trioctahedral mineral, and optionally a cationic coagulant. The polymer flocculant is added to the furnish after the fan pump and prior to the pressure screen; the inorganic particulate material is added to the furnish after the pressure screen, and optionally, the coagulant is added prior to the fan pump.

Description

Microparticle system in the papermaking process

Background of invention

Invention field

The microparticle system that the present invention relates to improve, and relate at the preparation paper product, promptly in paper or the cardboard microparticle system that improves is used as the method for auxiliary agent, wherein at retention, drainage, and paper formation (sheet formation) aspect has the performance of improvement.

The background technology explanation

In producing paper or cardboard, the rare Aquo-composition that is referred to as " batching " or " slurry " is sprayed onto on the mesh of the motion that is called " fourdrinier wire ".The solid constituent of said composition carries out drainage or filtration as cellulose fiber peacekeeping inorganic particles packing by fourdrinier wire, thereby forms page.Stay percentage of solids on the fourdrinier wire and be called " passing through retention first " in the papermaking process.

Retention it is believed that it is the function of different mechanism, as filtration by mechanical mist, and Electrostatic Absorption, and the bridge joint between fiber and the filler in the batching.Because the many fillers commonly used of cellulose fiber peacekeeping are all electronegative, therefore, they are to repel mutually.Usually, unique factor that can strengthen retention is mechanical mist.Thereby, use retention agent to improve fiber and the retention of filler on fourdrinier wire usually.

Drainage is relevant with the speed of removing moisture content when forming page from batching.The moisture that drainage only refers to usually after page forms and stands to be removed before any squeezing.Therefore, filter aid is used for improving total dewatering efficiency in paper or the production process.

The paper that evenness and paper-making process are produced or the evenness of cardboard are relevant.Usually, assess evenness by the variation of page iuuminting.Light transmission changes expression evenness " poor " greatly, and light transmission changes little ordinary representation evenness " good ".Usually, when retention increases, evenness usually will be poor from reducing to well.

Be understandable that, for various reasons,, improve retention in productivity ratio, dehydration rate, and the improvement of the evenness aspect of performance of final page or cardboard will be special hope.Good retention and good dehydration rate make the paper function move quickly, and reduce and shut down.Good paper formation will reduce the waste paper amount.Utilize retention agent and filter aid will realize these improvement.Retention agent and filter aid are: be used for making tiny solid material flocculation in the batching, so that improve the additive of these parameters in the paper-making process.The restriction of the flocculating effect when utilizing described additive to be subjected to paper sheet formation.If add more retention agent, so that the size of tiny solid coagulation of materials thing is increased, this will make the density of page change usually so, as mentioned above, and the paper formation that this may so-called with causing " poor ".Because overflocculation forms hole the most at last in page, and the water smoking in paper-making process subsequently will lose vacuum pressure, so this also can influence drainage.When being added in the batching at wet end of machine, retention agent and filter aid have three types usually, that is:

(a) single polymers;

(b) two-component polymer; Or

(c) microparticle system that can use with flocculant and/or coagulating agent.

As retention agent and filter aid, microparticle system can provide optimal results usually, and extensively describes in the prior art.The example of microparticle system publication comprises: EP-B-235, and 893, wherein together with high-molecular cationic polymer, the interpolation order with specific is used as inorganic matter with bentonite; WO-A-94/26972 has wherein described the vinyl amide polymer that uses with one of various inorganic matters and organic matter, described inorganic matter such as silica, bentonite, clay; WO-A-97/16598 has wherein described the kaolin that uses with one of various cationic polymers; And EPO805234, wherein use bentonite, silica or acrylate copolymer with the cationic dispersion polymer.

Comprise that bentonite is disclosed in the following document as the other microparticle system of inorganic matter: US4,749,444; 4,753,710; 4,913,775; 4,969,976; 5,126,014; 5,234,548; 5,393,381; 5,415,740; 5,514,249; With 5,532,308.These microparticle systems use: the flocculant and/or the coagulating agent that are added into wet end of machine with specific interpolation in proper order with inorganic material.

The microparticle system that comprises the water-swellable terre verte that uses with anionic polymeric dispersing agent is disclosed in US5, in 015,334.US5,071,512 has disclosed the microparticle system that uses hectorite with cationic starch.US5,178,730 have disclosed a kind of microparticle system, and this system comprises the hectorite that uses with medium or high-molecular cationic polymer.US5,194,120 have disclosed synthetic both sexes magnesium silicate, and for example LAPONITE is with the purposes of medium or high-molecular cationic polymer.With respect to one or more shear stage, for example purify, mix and pumping stage such as screen centrifuge, the votex hydrocyclone, mixing pump, and mixing pump, the each component of these microparticle systems all are added into the wet end of paper machine in proper order with specific interpolation.

The microparticle system of above-mentioned prior art, wherein some kinds are described as inorganic material with " bentonite " usually.Yet this term " bentonite " does not add qualification, therefore should not think usually to comprise saponite, more should not comprise hereinafter with the inorganic material of discussing.

Microparticle system comprises usually: contain or the not polymer flocculants of cation coagulating agent and tiny inorganic particulate pellet.The inorganic particulate pellet improves the efficient of flocculant and/or can produce littler, more uniform flocculate.

Although there are some kinds of microparticle systems in paper plant, to use at present, so that realize the paper performance of better paper machine operation performance and/or acquisition special-purpose, as the paper formation that improves for better printability, or the surface strength of improving; But still ten minutes is wished and is pressed for a kind of microparticle system, so that in paper-making process, improve the water filtering performance of paper or cardboard, and retention, and evenness performance.

Brief summary of the invention

The present invention has satisfied the demand.The present invention relates in paper-making process, be used as the microparticle system of retention agent and filter aid.

According to a first aspect of the invention, the invention provides a kind of production method of paper, described method comprises that the microparticle system that will be used as retention agent and/or filter aid is added in slurry or the batching; Described microparticle system comprises heavy polymer flocculant and inorganic particulate pellet, and wherein, the inorganic particle material package contains trioctahedron (trioctahedral) mineral matter that aluminium replaces, for example, and saponite.

According to a second aspect of the invention, the invention provides a kind of microparticle compositions that retention agent and/or filter aid are added into the improvement in paper pulp or the batching that can be used as, and described microparticle compositions comprises heavy polymer flocculant and inorganic particulate pellet, wherein, the inorganic particle material package contains the trioctahedron mineral that aluminium replaces, for example, saponite.

According to a third aspect of the invention we, the invention provides a kind of at retention, drainage and evenness aspect have paper or the board product that improves performance, wherein said paper or board product are added in aqueous cellulosic paper pulp or the batching by the microparticle system that will improve and make, wherein said microparticle compositions comprises heavy polymer flocculant and inorganic particulate pellet, and the inorganic particle material package contains the trioctahedron mineral that aluminium replaces, for example, and saponite.

A fourth aspect of the present invention relates to a kind of method for preparing paper or cardboard by forming the aqueous cellulosic paper furnish, and described method comprises:

(a) after first shear stage, the heavy polymer flocculant is added in the thin pulp stream of paper furnish, and after second shear stage, will comprise trioctahedron mineral that aluminium replaces for example saponite be added in the thin pulp stream of paper furnish;

(b) make the paper furnish drainage form page; With

(c) page is carried out drying.

Summary of drawings

Fig. 1 is the schematic diagram of illustrating a common paper machine part and the preferred point of addition of microparticle system each component of the present invention.

Fig. 2 illustrates drainage to the saponite consumption of polymer volume to saponite sample 1, the three-dimension surface of 5% the clay filler of first group of embodiment.

Fig. 3 illustrates drainage to the saponite consumption of polymer volume to saponite sample 1, the three-dimension surface of 20% the clay filler of first group of embodiment.

Fig. 4 illustrates drainage to the saponite consumption of polymer volume to saponite sample 2, the three-dimension surface of 20% the clay filler of first group of embodiment.

Fig. 5 is the two-dimensional diagram that the sample that comprises saponite and the turbidity of the sample that does not contain saponite are shown.

Fig. 6 is the drainage to embodiments of the invention 5-8 among second group of embodiment, MK evenness and the chart of having done by ash retention (FPAR%) result first.

Fig. 7 is the drainage to embodiments of the invention 9-12 among second group of embodiment, MK evenness and the chart of having done by ash retention (FPAR%) result first.

Detailed Description Of The Invention

The present invention relates in the paper-making process of acid and alkaline fine paper, particularly at the microparticle system of wet end of machine as retention agent and/or filter aid use.

Term " paper " comprises the product that comprises cellulosic sheet material as used herein, and they comprise page, cardboard etc.

Term " microparticle system or composition " refers to as used herein: the mixture of at least a hydrophilic polymer and at least a inorganic particulate pellet. The each component of described mixture can be added in pending slurry or the batching together, but preferably, individually and as described below order adds.

The present invention can utilize conventional paper machine to implement. Practice according to routine, batching or " thin pulp " that drainage forms page often make by the dilution underflow, described underflow usually in mixer or blending chest by with pigment or filler, suitable fiber, the reinforcing agent of any hope and/or other additive, and can be that the water of recycle-water mixes and makes. Claim slurry for example to use the vortex scummer to purify with the mode of routine. Usually, by purifying thin pulp by screen centrifuge. Usually, send described thin pulp by one or more centrifugal pump that is called mixing pump along the paper pump. For example, can thin pulp be pumped to screen centrifuge by the first mixing pump. Before the position that enters this first mixing pump or before this first mixing pump, the underflow dilutable water forms thin pulp, for example, and by making underflow and dilution water pass through mixing pump. By by the second screen centrifuge or pressurized screen, can further purify thin pulp, and before the one-tenth paper process of paper machine, pass through flow box.

The forming process of page can be utilized paper or the cardboard forming machine of any routine, flat long mesh paper making machine for example, and twin wire former, or any combination of cylinder former or these formers is finished. The flow apperach of paper machine (approach system) can comprise each assembly that is shown among Fig. 1. These assemblies comprise: mixing pump 1, pressurized screen 2, and flow box 3. Before entering mixing pump 1, by making underflow and dilution water by the mixing pump (not shown), water is diluted to thin pulp with underflow. By making thin pulp remove impurity in the thin pulp by pressurized screen 2, and before forming page, the thin pulp that leaves pressurized screen 2 is delivered in the flow box 3.

Fig. 1 has also illustrated the preferred point of addition of microparticle system each component of the present invention. Preferably, if use cationic coagulant,, by before the mixing pump 1 it is added in the thin pulp at thin pulp, thin pulp is along operation shown in the arrow 4, and point of addition is by arrow 5 expressions. When thin pulp is discharged mixing pump 1, flocculant is added into wherein, as by arrow 6 expressions, then when the thin pulp discharge pressure sieves 2, the inorganic particulate pellet is added into wherein, as being represented by arrow 7. Mixing pump 1, and pressurized screen 2 produces the shearing of height in the paper machine.

In the present invention, preferably, before the final position of thin pulp arrival high shear, add the high molecular weight flocculants polymer of microparticle system, and preferably, before the inorganic particulate pellet that adds microparticle system, resulting thin pulp is for example sheared at this final clipped position place. In Fig. 1, by adding before the pressurized screen 2, shown particulate adds after slurry passes through pressurized screen 2 shown flocculant at thin pulp.

Preferably, the flocculant of microparticle system of the present invention is added in the thin pulp (be that solid content wishes to be not more than 2%, or at the most 3% weight), rather than is added into underflow. Therefore, flocculant can be added directly in the thin pulp, in the dilution water that maybe can be added into to make underflow be transformed into thin pulp.

The high molecular weight flocculants polymer comprises solids, the especially preparation of subtitle substance cohesion that makes in the papermaking batching.Term " subtitle substance " means tiny solid particle and the fiber fines that defines in tappi test method T261 and T269 as used herein.

The flocculation of subtitle substance can be undertaken by heavy polymer itself in the batching, or combines with other formulation example such as high charge density cationic coagulant by heavy polymer and to carry out.The flocculation of subtitle substance will make the retention of subtitle substance in the fibre structure that forms page higher, improve dehydration or water filtering performance whereby.

The heavy polymer flocculant is: the polymer that flocculation preferably itself is provided.

The example that is applicable to heavy polymer flocculant of the present invention is a weight average molecular weight about 100,000 or higher, especially 500,000 or those higher flocculants.Preferably, molecular weight is about more than 1,000,000, and about more than 5,000,000 through being everlasting, for example 10,000,000 to 30,000,000 or higher scope in.These polymer can be: the linearity of acrylamide or other non-ionic monomer, side chain, cationic, non-ionic, both sexes, or the polymer of hydrophobically modified.

The amount that is added into the heavy polymer flocculant of the microparticle system in slurry of the present invention or the batching can be any amount that is enough to be present in to sening as an envoy to the obvious flocculation of solid, especially subtitle substance in slurry or the batching.The total amount of the water-soluble polymer that is added can be at about 0.0025wt% to about 1.0wt% scope, more preferably at 0.01wt% to about 0.2wt%, scope in, most preferably about 0.025wt% to about 0.1wt% (in be present in slurry or prepare burden in the dry weight of solid dry weight polymer).Interpolation can be carried out with one or many dosage at one or more point of additions, preferably, after the mixing pump that produces high shear forces, is added in the thin pulp stream with dose.

Desirable is before the inorganic particulate pellet that adds microparticle system, to make the flocculate that is formed by the heavy polymer flocculant stand shear action.Preferably, described shear action is produced by the pressurized screen that produces high shear forces.

Be added into the slurry in the inventive method or the amount of inorganic particulate pellet of the microparticle system in the batching, can be in the dry weight of existing solid about 0.005% to about 2.0% scope, preferably about 0.05% to about 0.5% scope.Though can add with one or many dosage in one or more positions, preferably add with dose, and preferably in Fig. 1 after the pressurized screen 2, and add the position between pressurized screen 2 and flow box 3 at least.

The inorganic particulate pellet of microparticle system of the present invention is preferably saponite, and it is the trioctahedron mineral that aluminium replaces.

Relating to retention, in the patent documentation of drainage and paper formation, mentioning many clay minerals, they include at " bentonite " or " swollen clay " or only are under " particulate " so wide title.Clay mineralogy is the field of a complexity, and as mentioned above, terminology often is not add to limit the ground use.Aforementioned US5,178,730 have discussed this problem in the 4th hurdle 14-32 is capable, comprising following content: " US4 for example, 753,710 have described bentonite and bentonite type clay as anion swollen clay, as sepiolite, Attagel, or montmorillonite preferably.This patent is also with reference to US4, wideer bentonite explanation (commercially available bentonite, imvite (montmorillonite clay), wyoming bentonite and bleaching earth) in 305,781.US4,749,444 have described bentonite, and as the sheet silicate of water-swellable, they comprise: nontronite, hectorite, saponite, wolchonskoite, sauconite, beidellite, rectorite (allevanite), illite, halloysite, Attagel and sepiolite.What accept usually in present clay mineralogy is taught book is, many in these mineral normally can not find in bentonite, and should not utilize bentonite that it is classified, for example some kinds of above-mentioned substances are not present in (allevanite in the terre verte family, illite, halloysite, attapulgite and sepiolite) and some of them are non-swelling (illite, attapulgite and sepiolites) ".

At aforementioned US5, in 178,730, actual " bentonite " refers to " dioctahedron " terre verte, and actual " hectorite " refers to and comprise natural " trioctahedron " terre verte that has clay.

The terre verte family of clay pit is normally: comprise the aluminium dioxide that is clipped between the two-layer silica octahedron or the three-layer mineral in the octahedra intermediate layer of magnesia.If middle octahedral layer comprises aluminum ions words, so, this smectic clays refers to " dioctahedron " mineral.If an octahedral layer comprises magnesium ion, this smectic clays refers to " trioctahedron " mineral so." isomorphous replacement " that smectite clay mineral is replaced by different atoms by the aluminium atom of silicon atom that is referred to as the certain percentage in two outer octahedral layers wherein and/or the certain percentage in middle octahedral layer or magnesium atom and specification configuration and chemical constituent.

" Alkaline minerals " of dioctahedron group is: the agalmatolite that does not have the isomorphous to replace in octahedral layer or tetrahedral layer.Owing to do not have internal layer CATION or water, so agalmatolite swelling not.Imvite, volchonskonite, beidellite and nontronite all drop in this agalmatolite group, wherein have different substitution values in three layers.

For example, imvite is characterised in that: have aluminium by some substitution values of magnesium (15-20% of about atomicity usually) in octahedral layer.Beidellite has in tetrahedral layer silicon by some substitution values of aluminium.Bentonite (Wyoming clay, bleaching earth) is: usually by the formed rock of pozzuolanic weathering, described volcanic ash mainly is imvite, and often comprises some beidellites.Nontronite has in octahedral layer aluminium by iron-based substitution value completely originally, and also have some in tetrahedral layer silicon by the substitution value of aluminium.Volchonskonite and nontronite are similar, but comprise chromium rather than iron in octahedral layer.The bentonite of most prior art documents is such smectic clays, promptly drops on usually in the scope of imvite.

" Alkaline minerals " for the trioctahedron group that does not contain isomorphous replacement in middle octahedral layer or the outer octahedral layer is talcum, and do not have any swollen performance as agalmatolite.Hectorite, saponite, sauconite, and usually also have vermiculite all to drop in the trioctahedron group.Hectorite has magnesium usually by some substitution values of lithium in middle octahedral layer.Saponite has some magnesium and also has some silicon by the substitution value of aluminium by the substitution value of aluminium and in outer octahedral layer in middle octahedral layer.In sauconite, main atom is zinc atom rather than magnesium atom in middle octahedral layer, and the some of them zinc atom is replaced by the aluminium atom, and the silicon atom in some outer octahedrons is replaced by the aluminium atom.Vermiculite has the silicon of height by the substitution value of aluminium or iron, and described aluminium or sheet iron strip have the magnesium cation of interlayer, and therefore, as described above those of most other naturally occurring terre vertes all have calcium or sodium cation at interlayer.At this employed term " saponite " be: the trioctahedral clay mineral that in middle octahedral layer and outer tetrahedron, has the aluminium substitution value.

Preferably, saponite is the inorganic particulate pellet of microparticle system of the present invention.Yet, it must be understood that the trioctahedron clay mineral that also can use other aluminium to replace is as sauconite and vermiculite.These trioctahedron mineral are different from hectorite wherein comprises the prior art of lithium substitution value in middle octahedral layer hectorite, be different from imvite, for example wherein imvite is the bentonite that has the prior art of the dioctahedron mineral of magnesium substitution value in the middle octahedral layer.

Add the high molecular weight flocculants polymer, will in slurry that adds polymer or batching, form the big flocculate of suspended solid usually.These big flocculates will be fractured in the prior art the very little flocculate that is referred to as " microfloc " immediately or subsequently by high shear forces.Described " high shear forces " can produce by the pressurized screen among Fig. 12 by the batching that makes flocculation.

Still with reference to figure 1, by being added in the underflow, preferably be added in the slurry before slurry is by mixing pump 1, the water-soluble polymer that its molecular weight is usually less than flocculant is as coagulating agent.Described coagulating agent is the cationic polymer of high charge density preferably, for example, if described coagulating agent polymer is the cationic nitrogenous polymer, its charge density in every kg of polymer nitrogen the gram equivalent more than 0.2, preferably at least 0.35, most preferably from 0.4-2.5 or higher.When this polymer carries out polymerization by CATION, ethylenically unsaturated monomer and other monomer and forms, the consumption of cationic monomer is to be used to form the used monomer total amount of polymer, usually at 2 moles more than the %, usually at 5 moles more than the %, preferably at least about 10 moles of %.

Suitable cationic coagulant comprises: inorganic aluminate, polyaluminium chloride (PAC), diallyl dimethyl ammoniumchloride (P-DADMAC); Poly-alkylamine; The cationic polymer of chloropropylene oxide and dimethylamine and/or ammonia or other primary amine and secondary amine; Polyamidoamines amine; Non-ionic monomer is as acrylamide, with cationic monomer, as the copolymer of DADMAC or acrylyl oxy-ethyl-trimethyl salmiac; The polymer of the cyanoguanidines modification of urea/formaldehyde resin; Melamine/yuban; Urea/yuban; Polymine; Cationic starch; Amphiphilic polymers with effective cationic charge; Mixture with above-mentioned coagulating agent.

The amount that is added into the cationic coagulant polymer of the microparticle system of the present invention in slurry or the batching can be to be enough to make the solid that is present in slurry or the batching to produce any amount of a large amount of coagulations.Being present in the dry weight of solid in slurry or the batching, total consumption of water-soluble coagulating agent polymer can be in the scope of about 0.0025wt% to 1.0wt%, more preferably at about 0.005wt% extremely in the scope of about 0.50wt%.

As mentioned above, cationic coagulant can be added in the underflow before mixing pump 1, the high molecular weight flocculants polymer can be added in the thin pulp after slurry is by mixing pump 1, and the inorganic particulate pellet can be added in the thin pulp after slurry is by pressurized screen 2.

Initial underflow can be according to the paper making pulp of any routine, and fiberfill that obtains according to cohesion or reuse method and composition thereof prepares; Described slurry is as according to traditional chemical pulp, for example bleaching and do not float sulfate pulp or sulfite pulp, and mechanical pulp such as ground wood pulp, thermomechanical pulp or CTMP, or reuse slurry are as deinked pulp.

The slurry of Shi Yonging in the methods of the invention, and final paper can be do not add substantially fill out (for example, in final paper, comprise be lower than 10% and be usually less than the filler of 5% weight), perhaps provide filler up to 50% at the dry weight meter of slurry solids, or in the paper dry weight up to 40% filler.When using filler, can there be the Chinese white filler of any routine, as calcium carbonate, kaolin, calcined kaolin, titanium dioxide or talcum, or its mixture.Filler (if present) and mixed before adding the microparticle system each component preferably in a usual manner.

The slurry of Shi Yonging can comprise the dispensable additive that other is known in the methods of the invention, as rosin, and alum, neutral sizing agent or optical brightener.Reinforcing agent or binding agent can also be comprised in addition, for example starch can be comprised, as cationic starch.PH value of slurry is usually from 4-9, and the special advantage of the inventive method is, low pH value for example pH be lower than at 7 o'clock, this method will be effective.

Fiber, filler, and the consumption of other additive such as reinforcing agent or alum all can be a conventional amount used.Usually, the solid content of thin pulp is from 0.1-3% weight, and perhaps fiber content is from 0.1-2% weight.Generally, the solid content of thin pulp is from 0.1-2% weight.

The inorganic particle material package of using in microparticle system of the present invention is drawn together: contain the clay material of trioctahedron aluminium, they are selected from saponite, volchonskonite, and terre verte, preferably saponite.In paper-making process, these particles are easy to be dispersed in the pulp-water suspension, so that strengthen the surface characteristic of final paper product.These particles have the dried average grain diameter less than 80 microns usually, and 1 micron to 10 microns typically, more typically from 2 nanometers to 2 micron, preferably from 1 nanometer to 1.2 micron.

Preferred average grain diameter is less than 1 micron particle, and described particle is present in the sizing agent before can be in being added into slurry, be broken into described particle size after perhaps can be in being added into slurry.Can conventional mode use conventional dispersant, water-soluble anionic polymer for example, as comprise the acidic polymer of acrylic acid groups or methacrylic acid group or its salt, for example, dry weight in the inorganic particulate pellet, add about 0.1% dispersant, so that assurance obtains the particle diameter of suitable fineness to about 3% weight.

We find, saponite (Na _0.9[Mg _5.0]) (Si _7.1Al _0.9) O ₂₀(OH ₄) can strengthen water filtering performance and retention with flocculant or flocculant/coagulating agent system, and in paper-making process, can improve the evenness of page.

Carry out two groups of laboratory tests below.For obtaining drainage and keep the result, first group is used flocculant and saponite, and the feeding position as shown in Figure 1.Be to obtain drainage, retention and paper formation result, second group use feeding shown in Figure 1 position be added into the flocculant in the thin pulp and the flocculant of saponite and feeding shown in Figure 1 position, coagulating agent, and saponite.

The following examples will be illustrated the present invention in more detail.These embodiment and not meaning that limit the scope of the invention.

Test-the first group

In first group embodiment, use following products:

Hydrocol 875 derives from Allied Colloids, the high molecular weight cation polyacrylamide polymer of Ltd.

Imvite 1016 derives from IMV Nevada (Amargosa Valley, dry soap stone clay NV).

SMI 200H-200mesh derives from GSA Resources, Inc (Tucson, Arizona) the dry soap stone clay of Yan Moing.

The Acme clay is to derive from ECC International Inc. (Roswell, Georgia) kaolin.

Embodiment 1

Pulp liquor

Preparation alkaline paper batching.Described batching is by comprising 80%Weyerhauser, and Prince AlbertHW paper pulp and 20% mixture of the Georgia Spectrum DP (Xerox level) of slurrying is again formed.Utilize laboratory scale Voith Allis Valley beater, batching is pulled an oar to the Canadian Standard Freeness (CSF) of 250ml, and be diluted to the concentration of 0.5% weight solid.The pH of slurries is maintained at about 7.8.Prepare two batches of such batchings.In the pulp liquor concentration expressed in percentage by weight, in first batching, add Acme clay as 5% weight of filler.In the pulp liquor concentration expressed in percentage by weight, in second batch of batching, add Acme clay as 20% weight of filler.

The preparation of preparation

The preparation of water-soluble polymer

Utilize magnetic stirring apparatus, at first Hydrocol 875 is mixed with the flow box concentration of 1.0wt%, be mixed with the concentration of 0.1wt% then in deionized water, for carrying out drainage and keeping that two batches of pulp liquors use in the test procedure with deionized water.

The preparation of saponite sample

In these embodiment of first group, make two kinds of saponite samples.SMI 200 H-200 purpose saponites are expressed as sample 1, and Imvite 1016 saponites are expressed as sample 2.

Saponite sample 1 and 2 each 5 gram are prepared with the 100ml deionized water and in the HamiltonBeach blender, mixed 15 minutes, be diluted to 1000ml with deionized water then.Utilize magnetic stirring apparatus again to sample 1 and sample 2 additional mixing 15 minutes and made it aquation at least 16 hours.As described below, in being added into pulp liquor before, respectively composite sample 1 and sample 2.

The drainage test

Utilize the Lightning mixer respectively the aliquot of 1 liter of pulp liquor first and second batch of material to be mixed in square container, described batch of material comprises the Acme clay filler of 5wt% and the Acme clay filler of 20wt% respectively.With constant airspeed 10 seconds (shear-mixed) when 1500rpm is of mixer.Above-mentioned polymer solution is added in these two kinds of pulp liquor batch of materials then, and under 1500rpm, stirred again one minute.Close mixer and slurries were shelved three minutes.

Saponite sample 1 is added in first batch of material of the batching that comprises 5wt% kaolin filler, and is added in second batch of material of the batching that comprises the 20wt% clay filler; Saponite sample 2 is added in second batch of material of the batching that comprises 20wt% kaolin filler.Between two beakers, topple over to and fro and comprise saponite, filler, and the final pulp liquor of polymer five times.Then the pulp liquor that obtains is poured in the drainage container, before pulp liquor carries out drainage, made drainage container vibration three times then.The water that filters is collected and is utilized for 30 seconds tared beaker to weigh then.Three final pulp liquors are carried out drainage test and map in Fig. 2-4.

Keep test

Turbidity

The turbidity of drainage can be the filler of system and measuring of subtitle substance retention.

Under 1500rpm, mix the batching batch of material 240ml (shear-mixed) that comprises 5wt% kaolin filler.When stirring, with the consumption of 6 pounds of dry polymerics of dried batching per ton polymer is added in the batching batch of material, and mixed for 15 seconds.Measurement comprise polymer solution and 5wt% filler batching drainage turbidity and map in Fig. 5 as sample 3.Then, with 12 pounds of dry soap stone of dried batching per ton consumption, saponite sample 1 is added in the batching.5 seconds of pulp liquor additional mixing to obtaining again.Measuring the turbidity of this batching also maps in Fig. 5 as sample 4.

Utilize Hach 2100P transmissometer to carry out turbidity test.

Handmade paper

The polymer solution of preparation is as mentioned above added in the other 240ml batching that comprises 5wt% kaolin filler.The dosage of sample 1 saponite solution is added in this batching and under 1500rpm mixed again for 5 seconds.These dosage are all listed in the table 1, and wherein dosage is respectively 6 pounds of dry polymerics of dried batching per ton and 0,6 and 12 pound of dry soap stone.

Table 1

Dosage	Retention
			6#/ton polymer 0#/ton saponite	????92.8％
6#/ton polymer 6#/ton saponite	????96.7％
		6#/ton polymer 12#/ton saponite	????100.0％

Utilize standard TAPPI mould and standard handmade paper step to prepare handmade paper.Preparation page and 500 ℃ of following ashing.In addition, also utilize and derive from Coors company (U.S.) and Whatman41 is housed the ceramic Bu Shi filter tunnel that does not have ash content filter paper and prepare pulpboard.

The drainage result

In showing that drainage is to the three-dimensional surface chart of dose of polymer to Fig. 2 of saponite (sample 1), the drainage data that first part of batch of material by the batching that comprises 5wt% kaolin filler obtains are mapped.Make dose of polymer do batching and change to 6.0 pounds of dry polymeric/tons and do batching, and make saponite (sample 1) dosage do batching to change to that 18 pounds of dry soap stone/tons are dried prepares burden from 0 pound of dry soap stone/ton from 1.2 pounds of dry polymeric/tons.By the chart of Fig. 2 as can be seen, when the dosage of polymer and saponite increases, water filtering performance will increase with the milliliter level.

Second batch of batching-20% clay filler-saponite sample 1

Fig. 3 illustrates the data of saponite sample 1, wherein, the drainage of the batching that comprises 20% clay filler is mapped to saponite dosage to dose of polymer.

Second batch of batching-20% clay filler-saponite sample 2

Fig. 4 illustrates the data of saponite sample 2, wherein, the drainage of the batching that comprises 20% clay filler is mapped to saponite dosage to dose of polymer.

With regard to Fig. 3 and Fig. 4, saponite dosage is done batching to 24 pounds of dry soap stone/tons from 0 pound of dry soap stone/ton and is done batching, and dose of polymer is that dried batching per ton is from 2.4-6.0 pound dry polymeric.

Here shown once more: when polymer and the increase of saponite dosage, water filtering performance will increase.

Keep the result

Turbidity can be measuring of retention.Higher turbidity represents that more fiber fines and filler are arranged in the drainage, thereby the retention of fiber fines and filler is just lower in paper.As mentioned above, the result to sample 3 and 4 maps in Fig. 5.

By the result of Fig. 5 mapping as can be seen, the turbidity that comprises the sample 4 of saponite and polymer is starkly lower than the turbidity of the sample 3 that does not contain saponite, and this shows: the retention that comprises the filler of sample of polymer and saponite and fiber fines is bigger.

Handmade paper

Test structure is all listed in the table 1.By the retention value of under 500 ℃, the ashing of handmade paper being measured filler.In addition, it can also be seen that in table 1: when being added into saponite in the batching, the retention of filler will increase.

Indicated as this first group test, the drainage of fiber fines and filler and retention can utilize two component particles systems, i.e. saponite and flocculant polymer and increase.

Second group of test

This group test will show: by comprising saponite and polymer flocculants, and so two components or the three component particles systems of dispensable coagulating agent, can increase the water filtering performance and the retention of fiber fines and filler.

Embodiment

The following examples will be illustrated the present invention in more detail.These embodiment in no case mean scope of the present invention are limited.Use following products in these embodiments:

Polymer A is to derive from (the Pittsburgh of Calgon company, PA) high molecular, cation acrylamide/acrylyl oxy-ethyl-trimethyl salmiac copolymer comprise about 90% mole acrylamide and about 10% mole acrylyl oxy-ethyl-trimethyl salmiac.

Polymer B is to derive from Calgon company (Pittsburgh, the homopolymers of intermediate molecular weight PA), diallyldimethylammonium chloride.

Polymer C is the high molecular weight cation acrylamide copolymer that derives from Ciba Specialty Chemicals, comprises about 25% cationic charge.

Hydrocol 2Dl is the dried bentonite that derives from Ciba Specialty Chemicals, i.e. montmorillonite.

Polymer D derives from Calgon company (Pittsburgh, the cationic polymer of PA), intermediate molecular weight, dimethylamine/chloropropylene oxide.

Polymer E derives from Calgon company (Pittsburgh, PA), high molecular, anion acrylamide copolymer comprises about 70% mol propylene acid amides and about 30% mol propylene acid.Polymer F derives from ECC International (Pittsburgh, polyaluminium chloride PA).

Polymer G be derive from ECC International (Pittsburgh, PA), acrylamide and diallyldimethylammonium chloride, intermediate molecular weight, cation copolymer.

Polymer H be derive from ECC International (Pittsburgh, PA), acrylamide, diallyldimethylammonium chloride and acrylic acid, intermediate molecular weight, terpolymer.

IMVITE 1016 derives from IMV Nevada (Amargosa Valley, dry soap stone NV).Carbital 60 be derive from ECC International (Atlanta, GA) do, powdered whiting.

Stalok 400 and Interbond C are the cationic starches that derives from A.E.Staley.

Hercon 70 is the AKD sizing agents that derive from Hercules Inc..

Embodiment 1-26

Embodiment 1-26 illustrates: different formulations of the present invention, and what synthesize, the water filtering performance of aqueous cellulosic batching, retention, and the improved validity in different page characteristics aspect, described page characteristic comprises evenness, brightness, and opacity.Described batching is designed to simulate the batching body paper that is used for preparing coating and uncoated magazine or printing and writes grade, typical alkaline, wood-free.

Preparation of batch

Utilize following each component preparation to be used for drainage and to keep test and be used to prepare the employed synthetic batching of handmade paper:

Fiber: 50/50wt% bleaching leaf wood kraft fibers/bleaching needlebush kraft fibers

Filler: 50/50wt% powdered whiting (Carbital 60)/winnofil

Amount of filler: fibre solid meter, 20wt%

Starch: in fibre solid, 0.5wt% (Interbond C)

Sizing agent: 0.25wt%Hercon 70 (AKD).

With the dry pulp plate soak in a tepid bath into the time 10 minutes, be diluted with water to the concentration of 2wt% solid then, and be refined to the Canadian Standard Freeness of 590ml with laboratory scale Valley beater.Starch, sizing agent and filler are added in the refining pulp liquor in proper order.The pH of pulp liquor is generally 7.5 ± 0.3.And then pulp liquor is diluted to the concentration of about 1.0wt% with running water, so that the thin pulp that is formed for testing.

The drainage test procedure

1. 200ml (the 2 gram solid) slurry of 1wt% flow box concentration is poured in the square mixer, and is diluted to 500ml with running water.

2. under the condition of following incorporation time and speed, utilize the Britt Jar type spiral shell blade-paddle mixer (1 inch diameter) of standard that inclusions is mixed, so that the simulation chemical agent is added into the inlet of second mixing pump, mixed pulp delivery side of pump, and the outlet of pressurized screen:

Time speed (rpm) additive feeding position

t ₀Before the 1200 coagulating agent mixing pumps

t ₁₀Before the 1200 flocculants sieve

t ₂₀Behind the 600 D/R/F auxiliary agents sieve

t ₃₀Stop

3. the inclusions of mixer is transferred in the drainage test tube of graduate of 500ml, the test tube bottom is equipped with 100 purpose screen clothes.With test tube counter-rotating 5 times, so that guarantee that slurry is even.Remove unstopper and measure 100ml, the elution time of 200ml and 300ml volume.For the blank test of the slurry that is untreated, the elution time of 300ml preferably should be greater than 60 seconds.

4. the drainage time with untreated blank sample is a benchmark, according to calculating as described below by the improvement of the water filtering performance provided is provided:

Drainability improves %=(untreated drainage time-handled drainage time) * 100/ untreated drainage time

Keep test procedure (FPR, FPAR, FPFR)

1. when stirring, the slurry of 500ml flow box concentration (1.0wt%) is poured in the Britt container that has 70 eye mesh screens with 1200rpm.

2. use the incorporation time/speed program identical with the drainage test procedure, so that simulation chemical agent point of addition and interpolation by the following step:

Time speed (rpm) additive feeding position

t ₀Before the 1200 coagulating agent mixing pumps

t ₁₀Before the 1200 flocculants sieve

t ₂₀Behind the 600 D/R/F auxiliary agents sieve

t ₃₀The 100ml eluent a. that opens the bottom cock and collect beginning filters this eluent by Whatman 4 filter papers and 105 ℃ of dry pad

Plate.At 500 ℃ of burning backing plates 2 hours to determine ash retention.

Handmade paper preparation and test

Use Noble ﹠amp; The Wood handsheet mold, preparation is the handmade paper of 70gsm quantitatively.This device will be produced the square handmade paper of 20cm * 20cm.The order of using in incorporation time/order that preparation is used in the handmade paper and drainage step is identical.Pour the batching sample of handling into Noble ﹠amp; In the deckle case of Wood handmade paper machine, and the standard technology that uses those skilled in the art to know prepares page.

The results are shown in table 2.

Table 2

	Before the mixing pump		Before the sieve		Behind the sieve		The filter pipe result	Pass through for the first time retention	Pass through for the first time ash retention	For the first time by the subtitle substance retention	M/K all spends	Brightness	Opacity
														Embodiment #	Product #1	Pound/ton	Product #2	Pound/ton	Product #3-	Pound/ton	Second/300ml	????(％)	????(％)	????(％)
????1	Blank	?????-	?-	????-	?????-	??-	????74	????79∶76	????17.75	????37.33	????23.0	?83.61	????72.77
														????2	????-	?????-	Polymer A	????0.1	??????-	???-	????59	????81∶44	????31.02	????42.53	????33.5	?84.28	????78.02
????3	????-	?????-	??″	????0.25	??????-	???-	????56	????84.80	????48.52	????52.92	????35.2	?84.80	????80.87
														????4	????-	?????-	???″	????0.50	??????-	???-	????47	????88.13	????63.43	????63.25	????33.8	?85.04	????83.29
????5	????-	?????-	???″	????0.75	??????-	??-	????41	????89.24	????70.14	????66.68	????30.9	?85.12	????85.35
														????6	????-	?????-	???″	????0.75	?IMVITE?1016	????3	????26	????91.54	????77.90	????73.81	????28.5	?84.93	????83.71
????7	????-	?????-	????″	????0.75	?????″	????6	????21	????90.30	????74.02	????69.97	????28.1	?85.08	????83.51
														????8	????-	?????-	???″	????0.75	??????″	????9	????20	????89.78	????71.82	????68.36	????28.9	?84.86	????85.78
????9	Polymer B	????0.1	???″	????0.75	??????″	????9	????19	????93.66	????84.73	????80.36	????27.1	?84.47	????86.30
														????10	?????″	????0.25	???″	????0.75	??????″	????9	????21	????95.58	????89.13	????86.32	????14.8	?84.17	????86.73
????11	?????″	????0.5	???″	????0.75	??????″	????9	????24	????97.55	????93.76	????92.40	????5.6	?83.61	????88.03
														????12	?????″	????1.0	???″	????0.75	??????″	????9	????39	????97.75	????93.88	????93.04	????3.2	?83.12	????82.92
????13	?????″	????0.5	???″	????0.75	??????″	????5	????33	????97.01	????92.33	????90.75	????6.5	?83.64	????86.20
														????14	?????″	????1.0	???″	????0.75	??????-	????-	????59	????93.53	????82.81	????79.97	????19.6	?83.62	????86.53
????15	?????″	????1.0	???″	????0.375	?IMVITE?1016	????5	????48	????95.65	????89.09	????86.52	????17.3	?83.59	????86.94
														????16	????″	????1.0	???″	????0.1	?????″	????9	????41	????91.71	????78.02	????74.32	????29.2	?83.78	????84.24
????17	????″	????1.0	???″	????0.1	????″	???-	????67	????86.45	????58.23	????58.03	????38.9	?83.67	????82.07
														????18	????″	????0.5	???″	????0.1	?IMVITE1016	????5	????44	????89.93	????72.06	????68.81	????38.9	?84.70	????85.49
????19	?????-	????-	??″	????0.1	??????″	????9	????52	????83.53	????47.52	????49.01	????38.3	?84.66	????80.41
														????20	?????-	????-	??″	???0.375	?????″	????5	????30	????87.14	????61.15	????60.18	????37.4	?84.87	????82.13
????21	Polymer B	????0.5	???″	???0.375	?????″	????5	????31	????94.87	????84.97	????84.11	????17.1	?84.41	????85.49
														????22	??????″	????0.5	???″	???0.375	?????″	????9	????26	????95.59	????87.77	????86.35	????13.5	?84.56	????85.10
????23	??????″	????0.5	???″	???0.375	?????-	????-	????57	????92.10	????77.30	????75.55	????29.2	?84.64	????83.81
														????24	??????″	????0.5	???″??	????0.1	?????-	????-	????60	????86.99	????59.91	????59.73	????43.1	?84.88	????84.56
????25	??????″	????0.25	???″	????0.1	?????-	????-	????59	????85.57	????52.96	????55.32	????43.0	?84.97	????82.96
														????26	?????″	????0.1	???″	????0.1	?????-	????-	????58	????84.09	????43.73	????50.73	????42.0	?84.61	????80.64

The embodiment 5-8 that maps in Fig. 6 shows: before pressurized screen polymer A and after the pressurized screen saponite with the simulation interpolation of 3-9 pound/ton dosage the water filtering performance of slurry will obviously be increased, and paper formation has only very little loss.To increase to maximum by ash retention (FPAR) when 3 pounds of/ton saponites first, and when high dose more, will reduce.

The embodiment 9-12 that maps in Fig. 7 shows: adding the 3rd component is cationic coagulant, to optionally improve first by ash retention (FPAR), and under the dosage of 0.1 pound of activating agent/ton at the most, drainability and paper formation almost do not change.When high dose more, FPAR will continue to increase, and water filtering performance will descend slightly, and paper formation will sharply descend.Not having under the saponite, shown in embodiment 14,17 and 23-26, water filtering performance and retention will obviously descend.

Table 3 and 4 shows the result of embodiment 27-50.

Table 3

	Before the mixing pump		Before the sieve		Behind the sieve		Water filtering performance
									Embodiment #	Product #1	Pound/ton activating agent	Product #2	Pound/ton activating agent	Product #2	Pound/ton activating agent	Second/300ml	% improves
????27	?????-	????-	???-	???-	???-	?-	????135	????0
									????28	Polymer B	????0.1	Polymer A	????0.5	?IMVITE1016	????1	????58	????57
????29	????“	????0.5	???“	????“	?????“	????1	????65	????52
									????30	?????“	????0.25	????“	????“	?????“	????3	????49	????64
????31	?????“	????0.1	?????“	????“	?????“	????5	????42	????69
									????32	?????“	????0.5	?????“	???“	??????“	????5	????47	????65
????33	?????-	???-	Polymer C	?0.3	?HydrocoI?2D1	????3	????102	????24
									????34	?????-	???-	????“	?0.3	?????“	????6	????99	????27
????35	?????-	????-	?????“	?0.6	??????“	????4.5	????81	????40
									????36	?????-	????-	?????“	?0.8	??????“	????3	????76	????44
????37	?????-	????-	?????“	?0.8	??????“	????6	????67	????50
									????38	Polymer D	????1	Polymer E	?0.4	The cataloid I	????0.8	????72	????47
????39	????“	????3	???“	?“	?????“	????0.8	????77	????43
									????40	????“	????2	???“	?“	?????“	????1.3	????65	????52
????41	?????“	????1	???“	?“	?????“	????1.8	????74	????45
									????42	????“	????3	???“	“	?????“	????1.8	????65	????52
????43	?Stalok?400	????8	?????-	???-	The cataloid I	????1.25	????75	????44
									????44	????“	????“	??-	???-	????“	????1.5	????67	????50
????45	????“	???“	??-	??-	????“	????2.0	????63	????53
									????46	Polymer F	????1	Polymer E	?0.5	????-	???-	????97	????28
????47	?????“	????3	??“	?0.5	????-	???-	????62	????54
									????48	?????“	????2	???“	?0.625	????-	????-	????74	????45
????49	?????“	????1	???“	?0.75	????-	????-	????91	????33
									????50	?????“	????3	???“	?0.75	????-	????-	????59	????56

Embodiment 27-50 in the table 3 compares water filtering performance of the present invention (embodiment 28-32) and conventional dual polymer scheme (embodiment 46-50) and cataloid (embodiment 38-42 and 43-45) and bentonite (embodiment 33-37) particulate scheme.For these schemes, when similar identical drainability, for being complementary with the prior art example, the present invention (embodiment 29) only needs total consumption of much less.In addition, as shown in table 4, when the paper formation value that can compare, of the present inventionly pass through ash retention first by what ash retention will be higher than prior art first.

Table 4

Embodiment #	Total program dosage (pound/ton)	Water filtering performance-improve %	FPAR(％)	MK evenness
					????29	????2.0	????52	????52	????20.6
????37	????6.8	????50	????49	????18.2
					????40	????3.7	????52	????20	????22.7
????45	????10.0	????53	????43	????18.8
					????47	????3.5	????54	????27	????21.6

Embodiment 51-77

The embodiment 51-77 of table 5 illustrates: different formulations of the present invention synthetic, aqueous formulations be at water filtering performance, retention, and the improved validity in different page characteristics aspect, and described page characteristic comprises evenness, brightness, and opacity.The component of described batching is to be used for preparing typical case's batching that lightweight coating level body paper is used.

Preparation of batch

Utilize following each component preparation to be used for drainage and to keep test and be used to prepare the employed synthetic batching of handmade paper:

Fiber: 45wt% bleaches leaf wood kraft fibers (SWK)/55wt% CTMP (CTMP)

Filler: calcined clay

Amount of filler: in dried fibre solid, 10wt%

Alum: in dried fibre solid, 0.5wt%

With CTMP be dipped in the hot water for the time 15-20 minute, in water, be diluted to the 1.56wt% solid concentration then, and be refined to the Canadian Standard Freeness of 200ml.Individually sulfate needle-leaved wood fibre (SWK) is dipped in the water, is diluted to 1.56wt%, and be refined to 550CSF.Fiber is sneaked in the preparation as mentioned above that contains the calcined clay filler then.Utilize dilute sulfuric acid conductance to be adjusted to 2000 μ S/cm with the pH regulator to 5.0 of mix and with sodium sulphate.

Table 5

	Before the mixing pump		Before the sieve		Behind the sieve
													Embodiment #	Product #1	Pound/ton	Product #2	Pound/ton	Product #2	Pound/ton	Drainage improves %	FPR( ％)	?FPA( ％)	MK evenness	Brightness	Opacity
????51	Poly-H	??0	Poly-A	?0.125	Saponite	????0	?19.1	?80.5	?37.5	?34.7	?60.9	?86.5
													????52	??“	??0	?“	?0.25	?“	????0	?37.6	?81.9	?45.7	?36.1	?61.4	?87.2
????53	???“	??0	?“	?0.375	?“	????0	?42.2	?82.4	?48.5	?35.2	?60.8	?88.5
													????54	???“	?1.5	??“	?0.125	??“	????0	?34.2	?82.4	?46.1	?33.2	?60.9	?87
????55	???“	?1.5	??“	?0.25	??“	????0	?40.6	?83.2	?48.5	?33.8	?60.8	?87.5
													????56	???“	?1.5	??“	?0.375	??“	????0	?46.2	?83.6	?49.9	?31.1	?61	?88.6
????57	???“	?3.0	??“	?0.125	??“	????0	?43.9	?82.8	?47.8	?32.2	?60.9	?88.1
													????58	???“	?3.0	??“	?0.25	??“	????0	?45.6	?83.2	?49.0	?30.7	?60.8	?88.4
????59	???“	?3.0	??“	?0.375	??“	????0	?52.7	?83.6	?52.7	?31.2	?61.1	?88.6
													????60	???“	??0	??“	?0.125	??“	??2.5	?31.4	?81.8	?45.0	?35.4	?61.2	?88.3
????61	???“	??0	??“	?0.25	??“	??2.5	?47.4	?82.1	?48.0	?33.5	?61.4	?88.6
													????62	???“	??0	??“	?0.375	??“	??2.5	?63.4	?83.3	?50.4	?29.8	?61.3	?88.4
????63	???“	?1.5	??“	?0.125	??“	??2.5	?55.8	?85.2	?55.3	?26.8	?61.4	?88.4
													????64	???“	?1.5	??“	?0.25	?“	??2.5	?62.8	?86.2	?59.2	?29.7	?60.8	?88.8
????65	???“	?1.5	???“	?0.375	?“	??2.5	?67.6	?87.2	?60.0	?27.3	?60.9	?88.9
													????66	???“	?3.0	???“	?0.125	?“	??2.5	?65.1	?86.0	?59.3	?22.1	?61	?89.2
????67	???“	?3.0	???“	?0.25	??“	??2.5	?66.4	?88.0	?64.2	?26.5	?61	?88.8
													????68	???“	?3.0	???“	?0.375	??“	??2.5	?69.9	?88.7	?66.3	?23.5	?60.9	?88.6
????69	???“	???0	??“	?0.125	??“	??5.0	?35.9	?82.2	?43.6	?31.6	?60.9	?87.7
													????70	??“	???0	?“	?0.25	??“	??5.0	?47.1	?83.2	?48.2	?25.7	?61.2	?88.5
????71	???“	???0	?“	?0.375	??“	??5.0	?59.5	?84.6	?52.9	?27.2	?61	?89.2
													????72	?“	?1.5	??“	?0.125	??“	??5.0	?63	?86.2	?59.3	?27.8	?61.1	?88.6
????73	?“	?1.5	??“	?0.25	??“	??5.0	?65.1	?87.0	?62.8	?30.1	?61	?88.9
													????74	?“	?1.5	??“	?0.375	??“	??5.0	?75	?87.0	?62.8	?21.8	?60.9	?89.1
????75	???“	?3.0	??“	?0.125	??“	??5.0	?69.9	?88.1	?67.1	?26.6	?60.9	?89.3
													????76	???“	?3.0	??“	?0.25	??“	??5.0	?75.7	?90.8	?72.1	?22.9	?60.9	?89.3
????77	???“	?3.0	?“	?0.375	?“	??5.0	?78.1	?90.1	?71.9	?19.3	?60.7	?89.7

Embodiment 78-110

The embodiment 78-110 of table 6 illustrates: different formulations of the present invention synthetic, aqueous formulations be at water filtering performance, retention, and the validity improved of paper formation aspect.The component of described batching is for being used for preparing the employed typical case's batching of cardboard.Under the similar identical situation of water filtering performance, compared with prior art, the present invention will provide obvious improvement first by ash retention and paper formation.

The batching preparation

Step preparation below utilizing is used for drainage and keeps test and be used to prepare the synthetic batching that handmade paper uses.

Decompose in warm water that 360 grams do not float, old corrugated board (OCC), and be diluted to 23 liters with deionized water.Paper pulp is refined to 300CSF.18 liters of described slurries are diluted to the concentration of 0.5wt% and add the salt of following consumption, so that the chemical of water is adjusted to suitable ionic strength (2000 μ S/cm):

A.5.61 restrain calcium chloride

B.0.96 restrain calcium chloride

C.8.17 restrain alum (50wt%)

D.15.96 sodium sulphate

E.0.59 restrain sodium bicarbonate

F.0.97 restrain sodium metasilicate

With dilute sulfuric acid with pH regulator to 5.0.

Table 6

	Before the mixing pump		Before the sieve		Behind the sieve
											Embodiment #	Product #	1	Pound/ton	Product #	2	Pound/ton	Product #	2	Pound/ton	Drainage improves %	FPR(％)	FPA(％)	MK evenness
????78	Polymer G	??0????	Polymer A	??0	Saponite	????0	????0	?80.5	?42.1	?20.8
											????79	??“	?1.5	???“	?0.12	????“	????2.5	????68	?91.8	?65.8	?15.8
????80	???“	?0.75	???“	?0.25	????“	????2.5	????67	?92	?57.9	?15.4
											????81	??“	?1.5	???“	?0.38	?????“	????0	????61	?91.5	?62.3	?17.0
????82	???“	?1.5	???“	?0.38	???“	????1.25	????69	?92.7	?60.5	?13.6
											????83	???“	?0	???“	?0.38	???“	????1.25	????64	?89.5	?56.1	?15.8
????84	???“	?0	???“	?0.12	???“	????1.25	????37	?87.7	?49.1	?18.4
											????85	???“	?0.75	???“	?0.12	???“	????2.5	????53	?90.4	?55.3	?17.4
????86	???“	?0	???“	?0.25	???“	????2.5	????53	?88.7	?51.8	?13.7
											????87	????“	?0	???“	?0.38	???“	????0	????58	?88.8	?50.9	?14.1
????88	????“	?1.5	???“	?0.12	???“	????0	????53	?89.6	?55.3	?14.7
											????89	???“	?1.5	???“	?0.25	???“	????1.25	????65	?91	?58.8	?11.1
????90	???“	?0.75	???“	?0.38	???“	????0	????51	?90.4	?59.7	?16.7
											????91	???“	?0	???“	?0.12	???“	????2.5	????32	?86.3	?40.4	?18.1
????92	????“	?0.75	???“	?0.12	???“	????1.25	????51	?89.5	?54.4	?15.9
											????93	???“	?0	???“	?0.12	???“	????0	????35	?86.9	?45.6	?18.2
????94	???“	?1.5	???“	?0.12	???“	????1.25	????60	?90.4	?51.8	?16.6
											????95	???“	?1.5	???“	?0.25	???“	????0	????57	?90.8	?70.2	?16.1
????96	????“	?0.75	???“	?0.25	???“	????1.25	????64	?90.1	?66.7	?13.2
											????97	???“	?1.5	???“	?0.38	???“	????2.5	????72	?93.2	?75.4	?15.9
????98	???“	?0.75	???“	?0.38	???“	????1.25	????69	?91.3	?71.9	?15.4
											????99	???“	?0.75	???“	?0.25	???“	????0	????55	?89.3	?64.9	?14.8
???100	???“	?1.5	???“	?0.25	???“	????2.5	????71	?92.4	?70.2	?14.2
											???101	???“	?0.75	???“	?0.25	???“	????1.25	????63	?89.8	?62.3	?14.2
???102	???“	?0.75	???“	?0.25	???“	????1.25	????60	?90.2	?64	?17.9
											???103	???“	????0	???“	?0.25	???“	????1.25	????51	?87.9	?58.8	?18.2
???104	???“	?0.75	???“	?0.12	???“	????0	????45	?88.0	?56.1	?19.0
											???105	???“	?0.75	???“	?0.25	???“	????1.25	????62	?90.8	?64.9	?15.6
???106	???“	?0	???“	?0.38	???“	????2.5	????62	?89.3	?57.9	?16.4
											???107	???“	?0.75	???“	?0.38	???“	????2.5	????72	?91.6	?65.8	?13.4
???108	???“	?0.75	???“	?0.25	???“	????1.25	????63	?89.9	?59.7	?17.0
											???109	???“	?0.75	???“	?0.25	???“	????1.25	????62	?89.4	?57.0	?15.5
???110	???“	?0	???“	?0.25	???“	????0	????49	?88.1	?57.9	?19.1

The embodiment 111-118 of table 7 compares the performance of the present invention of 100%OCC cardboard and the bentonite and the cataloid scheme of prior art.When identical water filtering performance, the present invention will provide the ash retention of obvious improvement, total retention, and paper formation (MK).

Table 7

Embodiment #	Scheme	Drainability improves (%)	First by ash retention (%)	First by retention (%)	MK evenness
						????111	The present invention	????37	????49.1	????87.7	????18.4
????112	???“	????63	????61.1	????89.9	????15.2
						????113	???“	????72	????70.5	????92.4	????14.5
????114	Bentonite	????34	????17.3	????85.9	????16.4
						????115	???“	????64	????35.8	????88.2	????14.1
????116	???“	????76	????49.4	????90.4	????12.6
						????117	Cataloid	????63	????34.6	????88.5	????12.4
????118	???“	????77	????54.3	????91.7	????13.6

Embodiment 119-145

The embodiment 119-145 of table 8 illustrates: different formulations of the present invention synthetic, aqueous formulations be at water filtering performance, retention, and the validity improved of different page characteristics aspect, and described page characteristic comprises evenness, brightness, and opacity.The component of described batching is the employed typical ground wood pulp batching of body paper that is used for preparing newsprint.

The batching preparation

Prescription below utilizing and step preparation are used for drainage and keep test and be used to prepare the employed synthetic batching of handmade paper.

Fiber: 80wt%CTMP/10wt%SWK/10wt% reuse newsprint

Filler: calcined clay amount of filler: in over dry solid 4wt%

Alum: 50 pounds/ton

pH：????4.8-5.2

Be immersed in CTMP in the hot water (140) and in mixer the disassociation 15-20 minute.Individually the reuse newsprint is dipped in the hot water and in mixer, dissociated 15-20 minute then.In warm water, the sulfate needle-leaved wood fibre was soaked 2 hours, and in mixer, dissociated 15-20 minute.According to the above ratio, with CTMP, the reuse newsprint, and the sulfate needle-leaved wood fibre mixes, and be refined to the CSF of 50-75ml in the concentration of 1.56wt%.With the calcined clay filler then alum be added in the slurry, make the pH of slurry be about 4.8-5.2.Utilize sodium chloride that the electric conductivity of slurry is adjusted to 2000 μ S/cm.

Table 8

	Before the mixing pump		Before the sieve		Behind the sieve
													Embodiment #	Product #1	Pound/ton	Product #2	Pound/ton	Product #2	Pound/ton	Drainage improves %	FPR( ％)	FPA( ％)	MK evenness	Brightness	Opacity
????119	Poly-H	?0	Poly-A	?0.063	Saponite	????0	?32.4	?73.4	?32.7	?20	?54	?98.7
													????120	?“	?0	?“	?0.156	??“	????0	??25	?76	?41.4	?21.3	?54.3	?98.7
????121	??“	?0	?“	?0.25	??“	????0	?38.3	?76	?39.8	?18.1	?54.1	?98.9
													????122	??“	?0.5	?“	?0.063	??“	????0	?32.4	?73.4	?32.7	?20	?54	?98.7
????123	??“	?0.5	??“	?0.156	??“	????0	?29.6	?75.1	?38.5	?17.7	?54.1	?98.8
													????124	??“	?0.5	??“	?0.25	??“	????0	?36.7	?76.2	?42.1	?15	?54.3	?99
????125	??“	?1.0	??“	?0.063	??“	????0	?32.4	?73.4	?32.7	????2	?54	?98.7
													????126	??“	?1.0	?“	?0.156	??“	????0	???-	?75	?36.9	?6.4	?54.3	?98.9
????127	??“	?1.0	??“	?0.25	??“	????0	?37.4	?76	?40.8	?15	?54.3	?99
													????128	??“	?0	?“	?0.063	??“	?1.3	???-	?77.9	?48.2	?23.1	?54.2	?99
????129	??“	?0	“	?0.156	?“	?1.3	?28.5	?75.9	?41.8	?17.5	?54.4	?98.8
													????130	??“	?0	?“	?0.25	?“	?1.3	?44.5	?77	?45.6	?12.6	?54.2	?99.2
????131	??“	?0.5	??“	?0.063	?“	?1.3	?32.6	?76.3	?45	?17.6	?54.3	?98.9
													????132	??“	?0.5	??“	?0.156	?“	?1.3	?44.7	?74.4	?37.9	?16.4	?54.3	?99
????133	??“	?0.5	??“	?0.25	?“	?1.3	?54.9	?73.2	?33.3	?13.9	?54.2	?99
													????134	??“	?1.0	??“	?0.063	?“	?1.3	???-	?75.5	?39.5	?16	?55	?99
????135	??“	?1.0	??“	?0.156	?“	?1.3	?51.6	?76.4	?43	?13.1	?54.2	?99
													????136	??“	?1.0	??“	?0.25	?“	?1.3	?56.5	?78.5	?49.6	?11.5	?54.1	?99.1
????137	??“	??0	?“	?0.063	?“	?2.5	?22.6	?73.6	?34	?19.4	?54.1	?98.6
													????138	??“	??0	?“	?0.156	?“	?2.5	???-	?76.7	?44.7	?17.3	?54.2	?99.1
????139	??“	??0	?“	?0.25	?“	?2.5	?52.7	?75.6	?39.5	?14.3	?54.2	?99.2
													????140	??“	?0.5	??“	?0.063	?“	?2.5	??-	?76.7	?45.9	?15.2	?54.4	?98.9
????141	??“	?0.5	??“	?0.156	?“	?2.5	?48.8	?76.5	?44.3	?12.8	?54.3	?99
													????142	??“	?0.5	??“	?0.25	?“	?2.5	??-	?80	?51.8	?11.8	?4.2	?99
????143	??“	?1.0	??“	?0.063	?“	?2.5	?51.1	?72.8	?31.1	?11.8	?54.3	?99
													????144	??“	?1.0	?“	?0.156	?“	?2.5	??-	?76	?44.3	?11.7	?54.2	?98.9
????145	??“	?1.0	??“	??0.25	?“	?2.5	?62.6	?79	?50.2	????9	?54.2	?99.1

During at basic identical water filtering performance with at maximum water filtering performance, the embodiment 146-150 of table 9 compares the prior art of performance of the present invention and typical newsprint batching.As shown in table 9, compared with prior art, the paper formation (MK) that the present invention will provide obviously higher maximum slurry water filtering performance and obviously improve when water filtering performance is basic identical, and obviously more during low production dosage page brightness significantly improve.

Table 9

	Before the mixing pump		Before the sieve		Behind the sieve
													Embodiment #	Product #	1	Pound/ton	Product #	2	Pound/ton	Product #	2	Pound/ton	Drainage improves %	FPR( ％)	?FPA( ％)	MK evenness	Brightness	Opacity
????146	Poly-H	1.0	Poly-A	?0.25	Saponite	2.5	?62.6	?79	?50.2	????9	?54.2	?99.1
													????147	?-	?-	??-	?0.25	???“	?1.3	?28.5	?75.9	?41.8	?17.5	?54.4	?98.8
????148	Poly-C	1.0	??-	??-	?Hydroc ?ol?2Dl	?7.0	?44.2	?85.5	?67.3	?3.8	?52.9	?99.1
													????149	Poly-C	1.0	??-	??-	?Hydroc ol?2Dl	?5.0	?26.7	?73.9	?62.5	?7.3	?53.2	?99.0
????150	?Stalok ?400	?20	Poly-E	?0.25	Cataloid	1.0	?22.5	?71.8	?25.6	?9.2	?53.0	?99.1

Embodiment 151

The application of industry paper machine, the lightweight coated paper

Producing 60 pounds/3300 feet ²Lightweight coating, contain on the industrial paper machine of wood fibre paper, performance of the present invention assessed, and with prior art in commercially available cataloid base scheme commonly used compare.For this assessment, polymer A is added into the porch of pressurized screen with the consumption of 0.2 pound of dry polymeric/dried ton paper, and saponite is added into the exit of pressurized screen with the consumption of 4 pounds of/ton dried paper.As shown in table 10, under identical machine speed, the invention provides the steam consumption of obvious improvement, paper formation, and pass through retention first.In addition, utilize the present invention, also obviously reduced the changeability of retention control and horizontal page humidity.

Table 10

Performance parameter	The present invention	Prior art
			Machine speed (fpm)	2100 (maximums)	2100 (maximums)
Backbone vapour pressure (psi)	????25	????28
			Paper formation (numerical value is low more good more)	????18	????20
First by retention (%)	????82	????78
			The horizontal humidity of page changes (pound, maximum to minimum)	????0.8	????1.2-1.5

Producing 40 pounds/3300 feet ²Lightweight coating, contain on the other industrial paper machine of wood fibre paper, also demonstrated validity of the present invention, and with prior art in commercially available cataloid base scheme commonly used compare.For this assessment, polymer A is added into the porch of pressurized screen with the consumption of 0.25 pound of dry polymeric/dried ton paper, and saponite is added into the exit of pressurized screen with the consumption of 4 pounds of/ton dried paper.As shown in table 11, under identical machine speed, the invention provides the steam consumption of obvious improvement, paper formation, flow box ash content concentration, and the brightness of page.

Table 11

Performance parameter	The present invention	Prior art
			Machine speed	????3300	????3300
Backbone vapour pressure (psi)	????11.7	????12.6
			Flow box ash content (%)	????13	????17
Page ash content (%)	????8.6	????8.65
			Paper formation (numerical value is low more good more)	????11.3	????12.0
Page brightness	????81.3	????80.2
			The page opacity	????77.4	????77.0

Embodiment 152

Industry paper machine application-liner board

On the industrial paper machine of producing double-deck liner board, performance of the present invention is assessed.Polymer A is added into the porch of pressurized screen with the consumption of 0.2-0.75 pound product/dried paper of ton.Saponite is added into the exit of pressurized screen with the consumption of 3-7 pound product/dried paper of ton.Increase to 86% by retention (FPR) from 63% first, and increase to 50% by ash retention (FPAR) from 10% first.Underflow liquid reduces 10-17%, and the solid amount that clarification and muddy branch line are held back descends 50%.

Above-mentioned " MK evenness " is: by the paper formation of M/K evenness tester measurement.

In order to describe, the present invention has described specific embodiment, but to those skilled in the art, it is evident that, under the situation of the present invention that in appended claims, defines, can make many changes and improvements to the present invention.

Claims (12)

1. a paper product that comprises retention agent and filter aid component is prepared burden, and comprises:

The heavy polymer flocculant, in the solid dry weight of described batching, its consumption from about 0.0025% to about 1.0% and

The inorganic particulate pellet that comprises the trioctahedron clay mineral of aluminium replacement, in the solid dry weight of described batching, its consumption from about 0.005% to about 2.0%.

2. the paper product of claim 1 is prepared burden, and also comprises in addition:

The cationic coagulant of high charge density, in the solid dry weight of described batching, its consumption from about 0.0025% to about 0.5%.

3. the paper product of claim 1 is prepared burden, and the trioctahedron clay mineral that wherein said aluminium replaces is selected from saponite, sauconite, and vermiculite.

4. the paper product of claim 3 is prepared burden, and the trioctahedron clay mineral that wherein said aluminium replaces is a saponite.

5. the production method of a paper product comprises following steps:

After the first high shear section and the second high shear section before, the heavy polymer flocculant is added in the batching, in the solid dry weight of described batching, its consumption from about 0.0025% to about 1.0% and

After the described second high shear section, the inorganic particulate pellet that will comprise the trioctahedron clay mineral of aluminium replacement is added in the batching, in the solid dry weight of described batching, and its consumption from about 0.005% to about 2.0%.

6. the method for claim 5 also comprises the steps: in addition

Before the described first high shear section, the cationic coagulant of high charge density is added in the batching, in the solid dry weight of described batching, its consumption from about 0.0025% to about 0.5%.

7. the method for claim 5, the trioctahedron clay mineral that wherein said aluminium replaces is selected from saponite, sauconite, and vermiculite.

8. the method for claim 7, the trioctahedron clay mineral that wherein said aluminium replaces is a saponite.

9. microparticle compositions that is suitable for use as retention agents and drainage agent in paper-making process, described composition comprises: heavy polymer flocculant and contain the inorganic particulate pellet of the trioctahedron clay mineral that aluminium replaces.

10. the composition of claim 9 also comprises the cationic coagulant of high charge density in addition.

11. the composition of claim 9, the trioctahedron clay mineral that wherein said aluminium replaces is selected from saponite, sauconite, and vermiculite.

12. the composition of claim 11, the trioctahedron clay mineral that wherein said aluminium replaces is a saponite.

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