CN103980420A - Preparation method of kaolin-based water-absorbing and water-retaining material - Google Patents
Preparation method of kaolin-based water-absorbing and water-retaining material Download PDFInfo
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- CN103980420A CN103980420A CN201410227255.1A CN201410227255A CN103980420A CN 103980420 A CN103980420 A CN 103980420A CN 201410227255 A CN201410227255 A CN 201410227255A CN 103980420 A CN103980420 A CN 103980420A
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Abstract
The invention discloses a preparation method of a kaolin-based water-absorbing and water-retaining material. The kaolin-based water-absorbing and water-retaining material can be applied to the fields of agriculture and forestry as well as the preparation of physical health and paper diaper resin materials. A gel prepared through a polymerization reaction of raw materials is cut into granules and dried in a microwave drying manner, wherein the drying process is finished within 10 to 30 minutes by controlling the content of volatile matters in the dried granules at 105 DEG C to be less than or equal to 10% and adjusting the service power of microwave equipment during the drying and the thickness of the gel cut into the granules during the drying. The adopted kaolin can be of kaolin (rock) raw powder, calcined kaolin powder or water-washed kaolin powder, wherein the powder fineness d97 is less than or equal to 45 microns. When the adopted kaolin is applied to the field of the preparation of the physical health and paper diaper resin materials, the whiteness of the calcined kaolin powder or the water-washed kaolin powder is greater than or equal to 85%; and the content of the kaolin is greater than or equal to 80%.
Description
Technical field
The present invention relates to a kind of preparation method of kaolin based water-absorbing-retaining material, a kind of a kind of method that is particularly related to kaolin based water-absorbing-retaining gel pelletizing microwave drying obtaining by polyreaction, moulding pelletizing, belongs to kaolin based water-absorbing-retaining resin material preparation field.
Background technology
At present, water-absorbing-retaining material can be widely used in many fields such as agricultural, Human Physiology health, paper nappy, oil, building, there is wide application market, but exist that resin material synthesis material cost is high always, gel particle time of drying longly makes the major defect that energy consumption is high, makes that water-absorbing-retaining material manufacturing cost is high and application causes larger disadvantageous effect to material large-scale popularization.
Employing has the function mineral of certain activity with the grafting of water-absorbing-retaining resin starting monomer, polymerization, is the effective way that reduces raw materials cost, and in this field, existing relatively large document and patent openly reported.But mineral compound water retaining agent prepared by actual prior art is still failed in agriculture, the large scale application of woods industry, though reason is because prior art has been improved the high present situation of raw materials cost, need removes 60% above water and cause the difficult problem that cost is higher but still fail the dry processing process of breakthrough solution water-absorbing-retaining material.
Dry main employing case (band) the formula forced air drying of the water-absorbing-retaining material gel that polymerization at present obtains and fluidizing fluid-bed dry, the process of its moisture removal is that first ecto-entad progressively carries out, in the outside moisture removal of gel, easily, at the fine and close colloid shell of the outside formation of gel, further hinder overflowing of internal moisture; The particularly dry this water-absorbing-retaining gelatinous material colloid large to water avidity, when form its internal moisture after colloid shell to remove difficulty larger.Gel as moisture 60% adopts 110 DEG C of box forced air drying processing, is dried to fugitive constituent and is less than 10%, and the general drying treatment amount time, more than 8h, exists large, the inefficient defect of energy consumption always.
Microwave technology is efficient power-saving technology, can be used for the field such as microwave radiation polymerization, microwave drying, and it is to having the distinguishing feature that the time is short, efficiency is high containing wet stock dry.Microwave technology is mainly the effect that has utilized microwave radiation polymerization in the application of water-absorbing-retaining material preparation field at present, the gel that obtains drying baker drying and dehydrating again after adopting alcoholic solvent to process.Between the Predominance Area of water-absorbing-retaining material polymerization preparation feedback temperature, it is the room temperature range at 15-30 DEG C, by adopting the control techniques of a small amount of initiator system to be easy to realize, use the larger microwave radiation device of equipment counter investment there is no significant technical superiority to polymerization process in this stage; Meanwhile, be wilkinite and attapulgite for the compound mineral of water-absorbing-retaining material preparation employing microwave radiation polymerization at present.
Water is the good transmitter substance of microwave, utilize microwave drying dehydration, its moisture overflow process is carried out from inside to outside, internal moisture first overflow the further passage that gel internal moisture removes of having expanded, and the surging force of internal moisture overflow process to gel pelletizing play " micro-explosion " effect, further increase drying and dehydrating and overflow area, drying process has the remarkable technical superiority that the time is short, energy consumption is low.As moisture 60% gel adopts microwave drying treatment, be dried to fugitive constituent and be less than 10%, the thickness when selecting microwave to use power and dried material, the treatment time, at 10min-30min, has the significant advantage that the time is short, efficiency is high, energy consumption is low.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of fast, the kaolin based water-absorbing-retaining resin material preparation method that efficient, energy consumption is low, its dry treatment process can be used for the preparation of the materials such as agricultural water-holding agent, physiological hygiene absorption agent and paper nappy absorption liquid resin.
The technical scheme that the present invention takes for technical solution problem is:
A kind of preparation method of kaolin based water-absorbing-retaining material, the gel granulated and dried of described polymerizable raw material reaction preparation adopts microwave drying, by controlling 105 DEG C of fugitive constituent≤10% of dry rear particle, thickness while adjusting the use power of microwave equipment when dry and gel granulated and dried, making time of drying is 10min-30min.
Described kaolin can be used the former powder of kaolin (rock), calcined kaolin powder, water-washed kaoline powder, its powder fineness d97≤45 μ m.
The raw material that described preparation is used and mass ratio are: kaolin 30-50, vinylformic acid 20-30, content 90% potassium hydroxide 13.9-20.8, acrylamide 40-90, (N, N)-methylene radical acrylamide 0.01-0.02, ammonium persulphate 0.05-0.20, azo diisobutyl amidine hydrochloride 0.03-0.06, sodium bisulfite 0.02-0.05, water 160-200
Described product is for physiological hygiene and paper nappy resin material field, preparing raw material used and mass ratio is: kaolin 10-30, vinylformic acid 40-50, content 95% sodium hydroxide 18.7-23.4, acrylamide 30-60, (N, N)-methylene radical acrylamide 0.01-0.02, ammonium persulphate 0.05-0.20, azo diisobutyl amidine hydrochloride 0.03-0.06, sodium bisulfite 0.02-0.05, water 150-180, the gel granulated and dried that it is characterized in that polymerizable raw material reaction preparation adopts microwave drying, by controlling 105 DEG C of fugitive constituent≤10% of dry rear particle, thickness while adjusting the use power of microwave equipment when dry and gel granulated and dried, making time of drying is 10-30min.
Described kaolin is calcined kaolin powder, water-washed kaoline powder, its whiteness >=85%, kaolinite content >=80%, powder fineness d97≤45 μ m.
beneficial effect of the present invention
1, the present invention can be used for agricultural, physiological hygiene and paper nappy resin material preparation field, the gel granulated and dried of polymerizable raw material reaction preparation adopts microwave drying, by controlling 105 DEG C of fugitive constituent≤10% of dry rear particle, thickness while adjusting the use power of microwave equipment when dry and gel granulated and dried, can complete at 10min-30min drying process.
2, water-absorbing-retaining material of the present invention has wide Application Areas and market capacity, overcomes and long etc. makes the defect that manufacturing cost is high existing high, the gel particle of raw materials cost time of drying in preparation.
3, water-absorbing-retaining material of the present invention has good water suction, water retention property, and cost is low, have great practical value, and is convenient to promote.
Embodiment
Embodiment 1
A preparation method for kaolin based water-absorbing-retaining material for agricultural, its step is as follows:
1., 160 parts of water are dropped in mixing kettles, start that under stirring, to add d97 be 30 parts, the former powder of kaolin of 45 μ m, stirring at room temperature is disperseed 20min, 20 parts of vinylformic acid is joined in mixing kettle, then stir, disperse 15min;
2., add 13.9 parts of the solid potassium hydroxide of content 90%, be no more than 50 DEG C with slurry temperature in mixing kettle and control potassium hydroxide feed rate, add again 40 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make dispersion, mixed slurry temperature lower than 30 DEG C afterwards, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 20min, continuing to add successively 0.01 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.03 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.05 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add afterwards 0.02 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 3h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 10min time of drying, dried particulate material through pulverize, screening, obtain 105 parts of moisture 10% finished products.
Embodiment 2
A preparation method for kaolin based water-absorbing-retaining material for agricultural, its step is as follows:
1., 200 parts of water are dropped in mixing kettles, start that under stirring, to add d97 be 50 parts, the calcined kaolin powder of 10 μ m, stirring at room temperature is disperseed 20min, after 30 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 18.7 parts of the solid potassium hydroxide of content 90%, be no more than 50 DEG C with slurry temperature in mixing kettle and control potassium hydroxide feed rate, add afterwards 90 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 30min, continuing to add successively 0.02 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.06 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.20 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.05 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 5h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 30min time of drying, dried particulate material through pulverize, screening, obtain 190 parts of moisture 7% finished products.
Embodiment 3
A preparation method for kaolin based water-absorbing-retaining material for agricultural, its step is as follows:
1., 180 parts of water are put into mixing kettle, start that under stirring, to add d97 be 40 parts, the water-washed kaoline powder of 45 μ m, stirring at room temperature is disperseed 20min, afterwards 25 parts of vinylformic acid is joined in mixing kettle, then stirs, disperses 15min;
2., add 17.3 parts of the solid potassium hydroxide of content 90%, be no more than 50 DEG C with slurry temperature in mixing kettle and control potassium hydroxide feed rate, add afterwards 70 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 25min, continuing to add successively 0.015 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.045 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.10 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.04 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 4h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 20min time of drying, dried particulate material through pulverize, screening, obtain 160 parts of moisture 9% finished products.
Embodiment 4
A preparation method for kaolin based water-absorbing-retaining resin material for physiological hygiene, its step is as follows:
1. 150 parts of water are put into mixing kettle, start that under stirring, to add d97 be 10 parts, the calcined kaolin powder of 12 μ m, whiteness 92%, kaolinite content 90%, stirring at room temperature is disperseed 20min, after 40 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 18.7 parts of the solid sodium hydroxides of content 95%, be no more than 50 DEG C with slurry temperature in mixing kettle and control sodium hydroxide feed rate, after add 30 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 20min, continuing to add successively 0.01 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.03 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.05 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.02 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 3h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 20min time of drying, dried particulate material through pulverize, screening, obtain 95 parts of moisture 8% finished products.
Embodiment 5
A preparation method for kaolin based water-absorbing-retaining resin material for physiological hygiene, its step is as follows:
1., 180 parts of water are put into mixing kettle, start that under stirring, to add d97 be 30 parts, the calcined kaolin powder of 45 μ m, whiteness 90%, kaolinite content 90%, stirring at room temperature is disperseed 20min, after 50 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 23.4 parts of the solid sodium hydroxides of content 95%, be no more than 50 DEG C with slurry temperature in mixing kettle and control sodium hydroxide feed rate, after add 60 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 30min, continuing to add successively 0.02 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.06 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.20 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.05 part of sodium bisulfite (being made into the 20g/ aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 5h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel and grain microwave drying, be 20min time of drying, dried particulate material through pulverize, screening, obtain 170 parts of moisture 10% finished products.
Embodiment 6
A preparation method for kaolin based water-absorbing-retaining resin material for paper nappy, its step is as follows:
1., 160 parts of water are dropped in mixing kettles, start that under stirring, to add d97 be 20 parts, the water-washed kaoline powder of 12 μ m, whiteness 88%, kaolinite content 85%, stirring at room temperature is disperseed 20min, after 40 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 18.7 parts of the solid sodium hydroxides of content 95%, be no more than 50 DEG C with slurry temperature in mixing kettle and control sodium hydroxide feed rate, after add 50 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 25min, continuing to add successively 0.015 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.045 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.10 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.03 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 4h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 10min time of drying, dried particulate material through pulverize, screening, obtain 130 parts of moisture 9% finished products.
Embodiment 7
A preparation method for kaolin based water-absorbing-retaining material for paper nappy, its step is as follows:
1., 180 parts of water are dropped in mixing kettles, start that under stirring, to add d97 be 30 parts, the water-washed kaoline powder of 45 μ m, whiteness 85%, kaolinite content 85%, stirring at room temperature is disperseed 20min, after 50 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 23.4 parts of the solid sodium hydroxides of content 95%, be no more than 50 DEG C with slurry temperature in mixing kettle and control sodium hydroxide feed rate, after add 60 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 30min, continuing to add successively 0.02 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.06 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.20 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.05 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 5h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 15min time of drying, dried particulate material through pulverize, screening, obtain 170 parts of moisture 10% finished products.
Embodiment 8
A preparation method for kaolin based water-absorbing-retaining material for paper nappy, its step is as follows:
1., 150 parts of water are dropped in mixing kettles, start that under stirring, to add d97 be 10 parts, the water-washed kaoline powder of 15 μ m, whiteness 86%, kaolinite content 80%, stirring at room temperature is disperseed 20min, after 45 parts of vinylformic acid are joined in mixing kettle, then stir, disperse 15min;
2., add 21.1 parts of the solid sodium hydroxides of content 95%, be no more than 50 DEG C with slurry temperature in mixing kettle and control sodium hydroxide feed rate, after add 45 parts of solid acrylamides, stirring and dissolving 15min, logical recirculated cooling water or liquid make mixed slurry temperature lower than 30 DEG C, and compound is squeezed into polymeric kettle;
3., logical nitrogen deoxygenation 20min, continuing to add successively 0.015 part of (N, N)-methylene radical acrylamide (being made into the 4g/L aqueous solution), 0.045 part of azo diisobutyl amidine hydrochloride (being made into the 10g/L aqueous solution), 0.10 part of ammonium persulphate (being made into the 20g/L aqueous solution) in logical nitrogen situation, continuing afterwards logical nitrogen 3min is uniformly dispersed slurry content, add again 0.03 part of sodium bisulfite (being made into the 20g/L aqueous solution), continue logical nitrogen 2-5min, stop logical nitrogen insulation reaction 4h;
4., logical pressurized air is by qualified reaction gel piece extrusion, pelletizing;
5., by gel pelletizing microwave drying, be 30min time of drying, dried particulate material through pulverize, screening, obtain 125 parts of moisture 8% finished products.
Claims (4)
1. the preparation method of a kaolin based water-absorbing-retaining material, it is characterized in that: the gel granulated and dried of described polymerizable raw material reaction preparation adopts microwave drying, by controlling 105 DEG C of fugitive constituent≤10% of dry rear particle, thickness while adjusting the use power of microwave equipment when dry and gel granulated and dried, making time of drying is 10min-30min.
2. the preparation method of a kind of kaolin based water-absorbing-retaining material according to claim 1, is characterized in that: described kaolin can be used the former powder of kaolin (rock), calcined kaolin powder, water-washed kaoline powder, its powder fineness d97≤45 μ m.
3. the preparation method of a kind of kaolin based water-absorbing-retaining material according to claim 1, it is characterized in that: the raw material that described preparation is used and mass ratio are: kaolin 30-50, vinylformic acid 20-30, content 90% potassium hydroxide 13.9-20.8, acrylamide 40-90, (N, N)-methylene radical acrylamide 0.01-0.02, ammonium persulphate 0.05-0.20, azo diisobutyl amidine hydrochloride 0.03-0.06, sodium bisulfite 0.02-0.05, water 160-200
The preparation method of a kind of kaolin based water-absorbing-retaining material according to claim 1, it is characterized in that: described product is for physiological hygiene and paper nappy resin material field, preparing raw material used and mass ratio is: kaolin 10-30, vinylformic acid 40-50, content 95% sodium hydroxide 18.7-23.4, acrylamide 30-60, (N, N)-methylene radical acrylamide 0.01-0.02, ammonium persulphate 0.05-0.20, azo diisobutyl amidine hydrochloride 0.03-0.06, sodium bisulfite 0.02-0.05, water 150-180, the gel granulated and dried that it is characterized in that polymerizable raw material reaction preparation adopts microwave drying, by controlling 105 DEG C of fugitive constituent≤10% of dry rear particle, thickness while adjusting the use power of microwave equipment when dry and gel granulated and dried, making time of drying is 10-30min.
4. the preparation method of kaolin based water-absorbing-retaining material for physiological hygiene according to claim 4 and paper nappy resin, it is characterized in that: described kaolin is calcined kaolin powder, water-washed kaoline powder its whiteness >=85%, kaolinite content >=80%, powder fineness d97≤45 μ m.
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