CN102635036A - Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent - Google Patents
Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent Download PDFInfo
- Publication number
- CN102635036A CN102635036A CN2012101362284A CN201210136228A CN102635036A CN 102635036 A CN102635036 A CN 102635036A CN 2012101362284 A CN2012101362284 A CN 2012101362284A CN 201210136228 A CN201210136228 A CN 201210136228A CN 102635036 A CN102635036 A CN 102635036A
- Authority
- CN
- China
- Prior art keywords
- sweet potato
- starch
- gram
- akd
- sexes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 244000017020 Ipomoea batatas Species 0.000 title claims abstract description 175
- 235000002678 Ipomoea batatas Nutrition 0.000 title claims abstract description 175
- 238000004513 sizing Methods 0.000 title claims abstract description 77
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- -1 Alkyl Ketene Dimer Chemical compound 0.000 title abstract description 3
- 229920001592 potato starch Polymers 0.000 title abstract 9
- 230000007935 neutral effect Effects 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 171
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000012188 paraffin wax Substances 0.000 claims abstract description 80
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 48
- 239000000839 emulsion Substances 0.000 claims abstract description 36
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000010525 oxidative degradation reaction Methods 0.000 claims abstract description 18
- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002472 Starch Polymers 0.000 claims description 174
- 239000008107 starch Substances 0.000 claims description 174
- 235000019698 starch Nutrition 0.000 claims description 174
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 239000007787 solid Substances 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 238000013019 agitation Methods 0.000 claims description 14
- 230000033228 biological regulation Effects 0.000 claims description 14
- 230000004927 fusion Effects 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- CSPHGSFZFWKVDL-UHFFFAOYSA-M (3-chloro-2-hydroxypropyl)-trimethylazanium;chloride Chemical class [Cl-].C[N+](C)(C)CC(O)CCl CSPHGSFZFWKVDL-UHFFFAOYSA-M 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000835 fiber Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000001804 emulsifying effect Effects 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- 241000209094 Oryza Species 0.000 description 21
- 235000007164 Oryza sativa Nutrition 0.000 description 21
- 235000009566 rice Nutrition 0.000 description 21
- 239000003292 glue Substances 0.000 description 19
- 244000085692 Cordia alliodora Species 0.000 description 8
- 235000004258 Cordia alliodora Nutrition 0.000 description 8
- 239000007844 bleaching agent Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000011436 cob Substances 0.000 description 7
- 239000010791 domestic waste Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 240000003183 Manihot esculenta Species 0.000 description 2
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 241000202567 Fatsia japonica Species 0.000 description 1
- 206010016590 Fibrin deposition on lens postoperative Diseases 0.000 description 1
- 241000276489 Merlangius merlangus Species 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Abstract
The invention discloses a preparation method of an amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent, which comprises the following steps of: firstly, carrying out oxidative degradation on the sweet potato starch under the action of hydrogen peroxide; carrying out cationization on the sweet potato starch subjected to the oxidative degradation by using 3-chloro-2-hydroxypropyltrimethyl ammonium chloride under the action of sodium hydroxide; then neutralizing by using acetic acid to obtain an amphiprotic sweet potato starch emulsifier; and finally emulsifying the AKD and paraffin wax by using the amphiprotic sweet potato starch emulsifier to obtain the amphiprotic sweet potato starch AKD neutral/alkaline sizing agent. The prepared amphiprotic sweet potato starch AKD neutral/alkaline sizing agent has positive charges and negative charges and is beneficial to tight combination with paper fibers, thus the sizing property is greatly improved. According to the invention, in a preparation process, amphiprotic sweet potato starch with low price is used as the emulsifier, and the paraffin wax with low price is used for replacing partial AKD with higher price, thus the stabilization property and sizing property of emulsion are improved, and the sizing cost is lowered.
Description
Technical field
The invention belongs to polymer chemistry sizing agent technical field, among particularly a kind of both sexes starch from sweet potato AKD/preparation method of alkaline sizing agent.
Background technology
The major progress of modern applying glue technology be in/popularization of alkaline bleach liquor sizing technology, during acid papermaking is converted into/alkaline paper-making is the great change on world's papermaking history.In/alkaline bleach liquor sizing is in papermaking process, the pH value is adjusted to more than 7, in principle without a kind of glue applying method of aluminum sulfate.In commonly used/alkaline sizing agent alkyl ketene dimer (being called for short AKD) is the product of phase late 1940s research and development; AKD be a kind of can with the response type of fibrin reaction in/alkaline sizing agent; It can be as internal sizing agent, again can be as Cypres.Its design feature is to be made up of active group and hydrophobic grouping; The fusing point of AKD is lower; Active group quaternary lactonic ring ability under the hot conditions of Dryer Section of Paper Machine in the molecule and the hydroxyl reaction on the cellulose form the beta-keto ester bond and are positioned on the fiber, and the hydrophobic group chain alkyl produces anti-water effect at fiber surface.Through among the AKD/alkaline bleach liquor sizing, the one way retention of paper whiteness, feel, WATER RESISTANCE, physical strength, printability, resistance to ag(e)ing and filler etc. all is significantly improved.And can to adopt cheap powdered whiting be filler, reduced content of harmful in the plain boiled water, improved the cyclic utilization rate of plain boiled water, and AKD is lower than the cost of acid accumulator size simultaneously.Adopt AKD carry out in/alkaline bleach liquor sizing can improve paper product quality and price, cut down the consumption of energy, improve environmental pollution and paper machine operation performance etc.; Therefore can obtain tangible economic benefit and social benefit, increasing papermaking enterprise is recognized and is used among the AKD/superiority and the necessity of alkaline sizing agent.China's paper making raw material is main with straw pulp, timber resource shortage, and the secondary stock consumption increases, in the utilization/the alkaline bleach liquor sizing technology has realistic meaning.Follow among the AKD/the alkaline bleach liquor sizing technology progressively enlarges in China's Application Areas; Technology is increasingly mature; In/benefit of alkaline paper-making progressively obtains embodying; Accelerated paper industry by acid papermaking in/trend that alkaline paper-making changes, in recent years AKD become domestic paper plant use at most, the most ripe, the most effectively in/alkaline sizing agent.
Among the AKD/alkaline bleach liquor sizing gives paper some excellent properties, and its weak point is also arranged simultaneously.Tradition AKD emulsion adopts the emulsifying agent of cassava cationic starch as AKD, and tapioca purity is high, and gelatinization point is low, sticks with paste the liquid good fluidity, a little less than transparency height, the retrogradation property, is difficult for layering.But its price is higher, and the AKD emulsion price that makes thus is higher, and the market competitiveness is poor.The research that improves in recent years and improve the AKD emulsion property is active day by day, improves the market competitiveness of AKD, among exploitation and production performance excellence, the low-cost AKD/and alkaline bleach liquor sizing is that China's papermaking researcher is made great efforts the problem studied always.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art; The object of the present invention is to provide among a kind of both sexes starch from sweet potato AKD/preparation method of alkaline sizing agent; In the gained/alkaline sizing agent has good stability, can improve the degree of sizing and the surface strength of paper, and reduce the applying glue cost.
For achieving the above object, the technical scheme that the present invention adopts is:
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; Water, starch from sweet potato, NaOH and hydrogen peroxide solution were added in first reactor 80-85 ℃ the time reaction 1.0-1.5 hour, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add NaOH and 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride then; Be warming up to 90-95 ℃ of reaction 1-2 hour, be cooled to 50-55 ℃ and add acetic acid, reduce to 20-30 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, the regulation system solid content promptly gets both sexes starch from sweet potato emulsifying agent to 20-25%,
The 3rd step added both sexes starch from sweet potato emulsifying agent, paraffin and AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature is to 70-75 ℃, treat paraffin and AKD fusion after, stirred 30-40 minute; The hot water that under agitation adds 75-80 ℃ disperses to be adjusted to solid content to 15-20%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 20-30MPa homogeneous; Be cooled to 25-30 ℃; Obtain solid content and be among the stable both sexes starch from sweet potato AKD of 15-20%/alkaline sizing agent, described paraffin is semi-refined paraffin wax or fully refined paraffin wax, or both are with the mixture of arbitrary proportion.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 65-70 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.0-3.5 kg/ton paper, the Cobb value of fluting medium is 35-40 gram/rice behind the Cypres
2, ring crush index is a 7.8-8.3 ox rice
2/ gram, fracture length is the 4.3-4.8 km, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, it is first that the applying glue cost of fluting medium per ton has reduced 7-12.
The present invention prepares and does not use the micromolecule surfactant in the process, helps the raising of environmental protection and effect.Earlier cationization is carried out in starch from sweet potato oxidative degradation then, it is applied to the emulsification of paraffin and AKD as emulsifying agent, in the preparation/the alkaline sizing agent emulsion viscosity is little, good stability.The emulsion particle of preparation is not only positively charged but also electronegative, helps to keep and can combine closely with electronegative paper fibre, not only improves emulsion-stabilizing performance and sizability, and has reduced the applying glue cost.
The specific embodiment
To be described in further detail the present invention with specific embodiment below.
Embodiment one
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 80 ℃ the time reaction 1.0 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 90 ℃ of reactions 2 hours, be cooled to 50 ℃ and add 5 gram acetic acid, reduce to 20 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 20% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 70 ℃, treat paraffin and AKD fusion after, stirred 40 minutes; The hot water that under agitation adds 75 ℃ disperses to be adjusted to solid content to 15%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 20MPa homogeneous, is cooled to 25 ℃; Obtain solid content and be among 15% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 65 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.0 kg/ton paper, the Cobb value of fluting medium is 40 gram/rice behind the Cypres
2, ring crush index is 7.8 Ns of rice
2/ gram, fracture length is 4.5 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 12 yuan.
Embodiment two
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 81 ℃ the time reaction 1.1 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 91 ℃ of reactions 1.8 hours, be cooled to 51 ℃ and add 5 gram acetic acid, reduce to 22 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 21% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 71 ℃, treat paraffin and AKD fusion after, stirred 38 minutes; The hot water that under agitation adds 76 ℃ disperses to be adjusted to solid content to 16%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 22MPa homogeneous, is cooled to 26 ℃; Obtain solid content and be among 16% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is fully refined paraffin wax.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 66 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.1 kg/ton paper, the Cobb value of fluting medium is 39 gram/rice behind the Cypres
2, ring crush index is 7.9 Ns of rice
2/ gram, fracture length is 4.6 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 11 yuan.
Embodiment three
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 82 ℃ the time reaction 1.2 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 92 ℃ of reactions 1.6 hours, be cooled to 52 ℃ and add 5 gram acetic acid, reduce to 24 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 22% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 72 ℃, treat paraffin and AKD fusion after, stirred 36 minutes; The hot water that under agitation adds 77 ℃ disperses to be adjusted to solid content to 17%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 24MPa homogeneous, is cooled to 27 ℃; Obtain solid content and be among 17% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 67 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.2 kg/ton paper, the Cobb value of fluting medium is 38 gram/rice behind the Cypres
2, ring crush index is 8.0 Ns of rice
2/ gram, fracture length is 4.7 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 10 yuan.
Embodiment four
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 83 ℃ the time reaction 1.3 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 93 ℃ of reactions 1.4 hours, be cooled to 53 ℃ and add 5 gram acetic acid, reduce to 26 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 23% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 73 ℃, treat paraffin and AKD fusion after, stirred 34 minutes; The hot water that under agitation adds 78 ℃ disperses to be adjusted to solid content to 18%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 26MPa homogeneous, is cooled to 28 ℃; Obtain solid content and be among 18% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is fully refined paraffin wax.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 68 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.3 kg/ton paper, the Cobb value of fluting medium is 37 gram/rice behind the Cypres
2, ring crush index is 8.1 Ns of rice
2/ gram, fracture length is 4.8 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 9 yuan.
Embodiment five
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 84 ℃ the time reaction 1.4 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 94 ℃ of reactions 1.2 hours, be cooled to 54 ℃ and add 5 gram acetic acid, reduce to 28 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 24% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 74 ℃, treat paraffin and AKD fusion after, stirred 32 minutes; The hot water that under agitation adds 79 ℃ disperses to be adjusted to solid content to 19%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 28MPa homogeneous; Be cooled to 29 ℃; Obtain solid content and be among 19% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax and fully refined paraffin wax mixture, and both mass ratioes are 2: 1.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 69 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.4 kg/ton paper, the Cobb value of fluting medium is 36 gram/rice behind the Cypres
2, ring crush index is 8.2 Ns of rice
2/ gram, fracture length is 4.9 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 8 yuan.
Embodiment six
Among a kind of both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 85 ℃ the time reaction 1.5 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 95 ℃ of reactions 1 hour, be cooled to 55 ℃ and add 5 gram acetic acid, reduce to 30 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 25% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 75 ℃, treat paraffin and AKD fusion after, stirred 30 minutes; The hot water that under agitation adds 80 ℃ disperses to be adjusted to solid content to 20%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 30MPa homogeneous; Be cooled to 30 ℃; Obtain solid content and be among 20% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax and fully refined paraffin wax mixture, and both mass ratioes are 1: 2.
With among this both sexes starch from sweet potato AKD/alkaline sizing agent is used for the 110 gram/rice of manufacturing paper with pulp with 100% domestic waste paper
2In the fluting medium, starch consumption 70 kg/ton paper, among the both sexes starch from sweet potato AKD/and alkaline sizing agent 3.5 kg/ton paper, the Cobb value of fluting medium is 35 gram/rice behind the Cypres
2, ring crush index is 8.3 Ns of rice
2/ gram, fracture length is 4.8 kms, reaches A level high-strength corrugated base paper QUALITY STANDARD, with among the both sexes starch from sweet potato AKD/the alkaline sizing agent applying glue after, the applying glue cost of fluting medium per ton has reduced by 7 yuan.
In sum, the present invention carries out cationization after adopting starch from sweet potato oxidative degradation, and it is applied to the emulsification of AKD and paraffin as emulsifying agent; Among the AKD of preparation/the alkaline sizing agent emulsion viscosity is little; Good stability, the emulsion particle of preparation is not only positively charged but also electronegative, helps to keep and can combine closely with electronegative paper fibre; Not only improve emulsion-stabilizing performance and sizability, and reduced the applying glue cost.
Claims (7)
1. among the both sexes starch from sweet potato AKD/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; Water, starch from sweet potato, NaOH and hydrogen peroxide solution were added in first reactor 80-85 ℃ the time reaction 1.0-1.5 hour, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add NaOH and 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride then; Be warming up to 90-95 ℃ of reaction 1-2 hour, be cooled to 50-55 ℃ and add acetic acid, reduce to 20-30 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, the regulation system solid content promptly gets both sexes starch from sweet potato emulsifying agent to 20-25%,
The 3rd step added both sexes starch from sweet potato emulsifying agent, paraffin and AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature is to 70-75 ℃, treat paraffin and AKD fusion after, stirred 30-40 minute; The hot water that under agitation adds 75-80 ℃ disperses to be adjusted to solid content to 15-20%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 20-30MPa homogeneous; Be cooled to 25-30 ℃; Obtain solid content and be among the stable both sexes starch from sweet potato AKD of 15-20%/alkaline sizing agent, described paraffin is semi-refined paraffin wax or fully refined paraffin wax, or both are with the mixture of arbitrary proportion.
2. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 80 ℃ the time reaction 1.0 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 90 ℃ of reactions 2 hours, be cooled to 50 ℃ and add 5 gram acetic acid, reduce to 20 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 20% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 70 ℃, treat paraffin and AKD fusion after, stirred 40 minutes; The hot water that under agitation adds 75 ℃ disperses to be adjusted to solid content to 15%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 20MPa homogeneous, is cooled to 25 ℃; Obtain solid content and be among 15% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax.
3. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 81 ℃ the time reaction 1.1 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 91 ℃ of reactions 1.8 hours, be cooled to 51 ℃ and add 5 gram acetic acid, reduce to 22 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 21% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 71 ℃, treat paraffin and AKD fusion after, stirred 38 minutes; The hot water that under agitation adds 76 ℃ disperses to be adjusted to solid content to 16%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 22MPa homogeneous, is cooled to 26 ℃; Obtain solid content and be among 16% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is fully refined paraffin wax.
4. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 82 ℃ the time reaction 1.2 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 92 ℃ of reactions 1.6 hours, be cooled to 52 ℃ and add 5 gram acetic acid, reduce to 24 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 22% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 72 ℃, treat paraffin and AKD fusion after, stirred 36 minutes; The hot water that under agitation adds 77 ℃ disperses to be adjusted to solid content to 17%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 24MPa homogeneous, is cooled to 27 ℃; Obtain solid content and be among 17% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax.
5. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 83 ℃ the time reaction 1.3 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 93 ℃ of reactions 1.4 hours, be cooled to 53 ℃ and add 5 gram acetic acid, reduce to 26 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 23% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 73 ℃, treat paraffin and AKD fusion after, stirred 34 minutes; The hot water that under agitation adds 78 ℃ disperses to be adjusted to solid content to 18%; Make both sexes starch from sweet potato AKD meta emulsion, the meta emulsion behind the 26MPa homogeneous, is cooled to 28 ℃; Obtain solid content and be among 18% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is fully refined paraffin wax.
6. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 84 ℃ the time reaction 1.4 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 94 ℃ of reactions 1.2 hours, be cooled to 54 ℃ and add 5 gram acetic acid, reduce to 28 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 24% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 74 ℃, treat paraffin and AKD fusion after, stirred 32 minutes; The hot water that under agitation adds 79 ℃ disperses to be adjusted to solid content to 19%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 28MPa homogeneous; Be cooled to 29 ℃; Obtain solid content and be among 19% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax and fully refined paraffin wax mixture, and both mass ratioes are 2: 1.
7. among a kind of both sexes starch from sweet potato AKD according to claim 1/and the preparation method of alkaline sizing agent, it is characterized in that, may further comprise the steps:
The first step; 200 gram water, 100 gram starch from sweet potato, 2 gram NaOH and 1 gram hydrogen peroxide solution were added in first reactor 85 ℃ the time reaction 1.5 hours, obtain the oxidative degradation starch from sweet potato, the mass ratio of water, starch from sweet potato, NaOH and hydrogen peroxide solution is 200: 100: 2: 1; In first reactor, add 7 gram NaOH and 49 gram 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides then; Be warming up to 95 ℃ of reactions 1 hour, be cooled to 55 ℃ and add 5 gram acetic acid, reduce to 30 ℃ again; The mass ratio of starch from sweet potato, NaOH, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride and acetic acid is 100: 7: 49: 5
Second step added water in first reactor, regulation system solid content to 25% promptly gets both sexes starch from sweet potato emulsifying agent,
The 3rd step added 120 gram both sexes starch from sweet potato emulsifying agents, 120 gram paraffin and 100 gram AKD in second reactor, wherein the mass ratio of both sexes starch from sweet potato emulsifying agent, paraffin and AKD is 120: 120: 100; Elevated temperature to 75 ℃, treat paraffin and AKD fusion after, stirred 30 minutes; The hot water that under agitation adds 80 ℃ disperses to be adjusted to solid content to 20%, makes both sexes starch from sweet potato AKD meta emulsion, with the meta emulsion behind the 30MPa homogeneous; Be cooled to 30 ℃; Obtain solid content and be among 20% the stable both sexes starch from sweet potato AKD/alkaline sizing agent, described paraffin is semi-refined paraffin wax and fully refined paraffin wax mixture, and both mass ratioes are 1: 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210136228.4A CN102635036B (en) | 2012-05-04 | 2012-05-04 | Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210136228.4A CN102635036B (en) | 2012-05-04 | 2012-05-04 | Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102635036A true CN102635036A (en) | 2012-08-15 |
| CN102635036B CN102635036B (en) | 2014-07-02 |
Family
ID=46619603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210136228.4A Expired - Fee Related CN102635036B (en) | 2012-05-04 | 2012-05-04 | Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102635036B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758517A (en) * | 2017-01-19 | 2017-05-31 | 中山联合鸿兴造纸有限公司 | A kind of page surface glue-applying technique method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007086803A1 (en) * | 2006-01-25 | 2007-08-02 | Stora Enso Ab | Sizing composition, method for the production of sized paper or paperboard and sized paper or paperboard |
| CN101759880A (en) * | 2010-01-13 | 2010-06-30 | 广东省造纸研究所 | Method for preparing amphiprotic starch solution for papermaking |
| CN102337707A (en) * | 2011-09-29 | 2012-02-01 | 浙江展航生物科技有限公司 | Preparation method of modified AKD (Alkyl Ketene Dimer) neutral sizing agent |
-
2012
- 2012-05-04 CN CN201210136228.4A patent/CN102635036B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007086803A1 (en) * | 2006-01-25 | 2007-08-02 | Stora Enso Ab | Sizing composition, method for the production of sized paper or paperboard and sized paper or paperboard |
| CN101759880A (en) * | 2010-01-13 | 2010-06-30 | 广东省造纸研究所 | Method for preparing amphiprotic starch solution for papermaking |
| CN102337707A (en) * | 2011-09-29 | 2012-02-01 | 浙江展航生物科技有限公司 | Preparation method of modified AKD (Alkyl Ketene Dimer) neutral sizing agent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758517A (en) * | 2017-01-19 | 2017-05-31 | 中山联合鸿兴造纸有限公司 | A kind of page surface glue-applying technique method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102635036B (en) | 2014-07-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102660897B (en) | Preparation method for highly-dispersed cationic AKD (Alkyl Ketene Dimer) as neutral/alkali sizing agent | |
| CN102635033B (en) | Preparation method of no-sizing lag beewax/AKD (alkyl ketene dimer) neutral/alkaline sizing agent | |
| CN102635030B (en) | Preparation method for cation corn starch alkyl ketene dimer (AKD) neutral/basic sizing agent | |
| CN102635025B (en) | Preparation method of amphiprotic corn starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102627734B (en) | Preparation method of amphoteric alkyl ketene dimer (AKD) neutral/alkaline sizing agent without sizing lag | |
| CN102635029A (en) | Preparation method of cation sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102627732A (en) | Preparation method of high-activity half-crosslinking alkyl ketene dimer (AKD) neutral/alkaline sizing agent | |
| CN102635036B (en) | Preparation method of amphiprotic sweet potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102660901B (en) | Preparation method for sizing-free curing time semi-crosslinked AKD (Alkyl Ketene Dimer) as neutral/alkali sizing agent | |
| CN102635028B (en) | Preparation method for cation sweet potato starch microcrystalline wax/alkyl ketene dimer (AKD) neutral/basic sizing agent | |
| CN102660900B (en) | Preparation method of amphoteric corn starch microcrystalline wax/AKD (alkyl ketene dimer)/alkaline sizing agent | |
| CN102635031B (en) | Preparation method for cation potato starch microcrystalline wax/alkyl ketene dimer (AKD) neutral/basic sizing agent | |
| CN102635035B (en) | Preparation method of amphiprotic potato starch AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102660899B (en) | Method for preparing cation potato starch alkyl ketene dimer (AKD) neutral/alkaline sizing agent | |
| CN102635037B (en) | Preparation method of amphoteric sweet potato starch microcrystalline wax/ AKD (alkyl ketene dimer) neutral /alkaline sizing agent | |
| CN102660904B (en) | Preparation method for amphiprotic potato starch microcrystalline wax/AKD (Alkyl Ketene dimer) neutral/alkaline sizing agent | |
| CN102635026B (en) | Preparation method for sizing curing time-free alkyl ketene dimer (AKD) neutral/basic sizing agent | |
| CN102635027B (en) | Preparation method of cation corn starch microcrystalline wax/AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102660898B (en) | Preparation method for highly-dispersed semi-crosslinked AKD (Alkyl Ketene Dimer) as neutral/alkali sizing agent | |
| CN102635032B (en) | Preparation method of sizing lag-free semi-crosslinked AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102635034B (en) | Preparation method of sizing curing time-free beewax/AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent | |
| CN102635015B (en) | Preparation method for cation high-dispersion semi-crosslinking alkyl ketene dimer (AKD) neutral/basic sizing agent | |
| CN102627736B (en) | Preparation method for alkyl ketene dimmer (AKD) neutral/alkali sizing agent without sizing lag | |
| CN102627738B (en) | Preparation method for amphiprotic alkyl ketene dimmer (AKD) neutral/alkali sizing agent without sizing maturation period | |
| CN102635022B (en) | Preparation method of high-activity ceresin/AKD (Alkyl Ketene Dimer) neutral/alkaline sizing agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201224 Address after: 224000 Qingyang Road (within Qingdun Office), Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (8) Patentee after: Yancheng Qinglong Jinbang water Co.,Ltd. Address before: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. Effective date of registration: 20201224 Address after: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right | ||
| CI03 | Correction of invention patent |
Correction item: Patentee|Address Correct: Yancheng Qingdun Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) False: Yancheng Qingyi Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) Number: 02-01 Volume: 37 |
|
| CI03 | Correction of invention patent | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140702 |