CN105273666A - Method for preparing composite biomass adhesive by using papermaking black liquor - Google Patents
Method for preparing composite biomass adhesive by using papermaking black liquor Download PDFInfo
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Abstract
The invention discloses a method for preparing a composite biomass adhesive by using papermaking black liquor and belongs to the technical field of adhesives. The method comprises the steps of firstly pretreating the papermaking black liquor so as to remove large-grained impurities from the papermaking black liquor, then, mixing the papermaking black liquor with glacial acetic acid, polyacrylamide and the like so as to obtain a lignin-containing mixture, mixing the lignin-containing mixture with ammonia water, dimethylformamide and the like so as to obtain a modified lignin mixture, stirring the modified lignin mixture with starch, putting the mixture into a vessel, adding substances such as ammonium persulfate and N,N-dimethylformamide into the vessel, and carrying out reaction, thereby obtaining the composite biomass adhesive. Proven by examples, sheet material finished products made by using the adhesive prepared by the method are environment-friendly and safe, the content of free formaldehyde measured finally is decreased to 0.8-1.2% from 5-7%, and the removal ratio reaches up to 84% or more; and the papermaking black liquor serves as a raw material, and the waste is utilized, so that the cost is reduced, the environment is protected, and all indexes detected reach national standards.
Description
Technical field
The invention discloses a kind of method utilizing black liquid to prepare composite biomass sizing agent, belong to sizing agent technical field.
Background technology
China is the country of Shaolin, there is larger contradiction between timber supply and demand, solves the important channel of this contradiction, is production and the utilization of the composite sheet must greatly developed centered by wood-based plate.Produce 1 cubic metre of shaving board with urea-formaldehyde resin adhesive, the sheet material that 3.2 cubic metres of logs are made can be replaced; And produce 1 ton of fiberboard with urea-formaldehyde resin adhesive, 5.3 cubic metres of log panels can be replaced.Namely tackiness agent is significant to raising timber utilization rate; Meanwhile, timber industry is also huge to the consumption of tackiness agent, in the composite sheets such as wood-based plate, glued board, sandwich panel, cored slab, sewing machine table, wood plastic composite, wooden alloy sheets, all will adopt a large amount of tackiness agent.Such as: produce 15000 cubic metres of glued boards and need tackiness agent 1500 tons.
As can be seen here, a large amount of sizing agents to be consumed in the production of composite sheet, and to use maximum in these sizing agents be urea-formaldehyde resin adhesive, it has good adhesiveproperties, its sticky strong strength ratio animal and plant glue is high, the viscose glue that photostabilization is good and be applicable to the composite sheets such as timber, glued board, veneer sheet and bamboo and wood products is produced, and the more important thing is that its price comparison is low and is widely used.And these composite sheet goods are widely used in the place such as family and office that people hang up one's hat, live.But, a certain amount of free formaldehyde is there is in these sizing agents or composite sheet goods, such as, free formaldehyde content in urea-formaldehyde resin adhesive is up to 5 ~ 7%, because of its-formaldehyde that give off poisonous gas in process for processing and use procedure, severe contamination infringement people's is healthy, and use should be very restricted.But, still also effectively cannot limit it at present and use, and develop into uncontrollable situation.Therefore, develop, application low formaldehyde content composite sheet sticks with glue agent becomes the task of top priority, and seem very necessary.
Summary of the invention
The technical problem that the present invention mainly solves: what the sizing agent for current industrial application was maximum is urea-formaldehyde resin adhesive, although its adhesiveproperties, photostabilization are relatively good, but formaldehyde can be given off poisonous gas in production or use procedure, pollute environment, compromise the problem of HUMAN HEALTH, provide a kind of method utilizing black liquid to prepare composite biomass sizing agent.The method is first by carrying out pre-treatment to black liquid, remove large granular impurity wherein, then it is mixed with Glacial acetic acid, polyacrylamide etc., obtain the mixture containing xylogen, itself and ammoniacal liquor, dimethyl formamide etc. are being mixed to get modified lignin resin mixture, modified lignin resin mixture and starch are stirred, put into container, add the material such as ammonium persulphate, DMF wherein, react, obtain composite biomass sizing agent.The sizing agent Environmental Safety not only made, the formaldehyde not containing any harmful to human exists, and is starting material with black liquid, and utilization of waste material, reduces cost, protects environment.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) get 1 ~ 3L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.0 ~ 7.5, be heated to black liquid boiling, keep temperature 1 ~ 3h, then add 100 ~ 300mL absolute ethyl alcohol and stirring wherein even, filter after leaving standstill 30 ~ 40min;
(2) by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 100 ~ 300g polyacrylamide wherein and 200 ~ 300mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate;
(3) be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 140 ~ 230mL dimethyl formamide more wherein to stir, leave standstill after 15 ~ 25min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture;
(4) the modified lignin resin mixture getting 300 ~ 400g gained puts into container, add 50 ~ 80g starch wherein, mix, then add 150 ~ 180g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 4 ~ 8%, container is placed in water-bath to carry out being heated to 60 ~ 70 DEG C, after stirring 1 ~ 3h, add 150 ~ 200mL vinyl acetate wherein, still aging 5 ~ 10h;
(5) after above-mentioned standing end, 130 ~ 170mL4-tertiary butyl phenol is added respectively wherein, 80 ~ 120mL massfraction is the sodium hydroxide solution of 60%, after stirring 30 ~ 40min, add 60 ~ 90mL Myracaldehyde wherein again, be warming up to 80 ~ 90 DEG C, add 50 ~ 100g zinc oxide and carry out catalysis, use nitrogen to protect, stir 1 ~ 3h;
(6) after above-mentioned stirring terminates, be down to room temperature, add 30 ~ 60g silane coupling agent wherein, stir, and then add 40 ~ 80g urea wherein, at temperature is 68 ~ 78 DEG C, after stirring 30 ~ 40min, be down to room temperature, composite biomass sizing agent can be obtained.
Application method of the present invention is: during use, and biomass sizing agent the present invention made is poured into after on spreadometer, and during dry finishing is good, plate is delivered on spreadometer and carried out gluing, and Amount of spread controls at 100 ~ 120g/m
2afterwards plate in glue-coated multilayer is loaded on preformer and carry out precompressed, hot pressing on thermocompressor is put into again after precompressed, arranging hot pressing pressure is 4 ~ 8MPa, and hot pressing temperature is 110 ~ 145 DEG C, takes out after hot pressing 10 ~ 15s, finally sheet material finished product is detected, record free formaldehyde content and be reduced to 0.8 ~ 1.2% from 5 ~ 7%, clearance, up to more than 84%, reaches the requirement of premium grads.
The invention has the beneficial effects as follows:
(1) the sizing agent Environmental Safety made of the present invention, adhesive effect is remarkable, and the formaldehyde not containing any harmful to human exists, for environment without any harm;
(2) the present invention take black liquid as starting material, and utilization of waste material, reduces production cost, protects environment.
Embodiment
First get 1 ~ 3L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.0 ~ 7.5, be heated to black liquid boiling, keep temperature 1 ~ 3h, then add 100 ~ 300mL absolute ethyl alcohol and stirring wherein even, filter after leaving standstill 30 ~ 40min; Then by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 100 ~ 300g polyacrylamide wherein and 200 ~ 300mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate; Be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction subsequently, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 140 ~ 230mL dimethyl formamide more wherein to stir, leave standstill after 15 ~ 25min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture;
Next the modified lignin resin mixture getting 300 ~ 400g gained puts into container, add 50 ~ 80g starch wherein, mix, then add 150 ~ 180g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 4 ~ 8%, container is placed in water-bath to carry out being heated to 60 ~ 70 DEG C, after stirring 1 ~ 3h, add 150 ~ 200mL vinyl acetate wherein, still aging 5 ~ 10h;
130 ~ 170mL4-tertiary butyl phenol is added respectively wherein again after above-mentioned standing end, 80 ~ 120mL massfraction is the sodium hydroxide solution of 60%, after stirring 30 ~ 40min, add 60 ~ 90mL Myracaldehyde wherein again, be warming up to 80 ~ 90 DEG C, add 50 ~ 100g zinc oxide and carry out catalysis, use nitrogen to protect, stir 1 ~ 3h; Last after above-mentioned stirring terminates, be down to room temperature, add 30 ~ 60g silane coupling agent wherein, stir, and then add 40 ~ 80g urea wherein, at temperature is 68 ~ 78 DEG C, after stirring 30 ~ 40min, be down to room temperature, composite biomass sizing agent can be obtained.
Example 1
First get 1L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.0, be heated to black liquid boiling, keep temperature 1h, it is even then to add 100mL absolute ethyl alcohol and stirring wherein, filters after leaving standstill 30min; Then by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 100g polyacrylamide wherein and 200mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate; Be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction subsequently, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 140mL dimethyl formamide more wherein to stir, leave standstill after 15min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture; Next the modified lignin resin mixture getting 300g gained puts into container, add 50g starch wherein, mix, then add 150 ~ 180g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 4%, container is placed in water-bath to carry out being heated to 60 DEG C, after stirring 1h, add 150mL vinyl acetate wherein, still aging 5h; After above-mentioned standing end, add 130mL4-tertiary butyl phenol respectively wherein again, 80mL massfraction is the sodium hydroxide solution of 60%, after stirring 30min, add 60mL Myracaldehyde wherein again, be warming up to 80 DEG C, add 50g zinc oxide and carry out catalysis, use nitrogen to protect, stir 1h; Finally after above-mentioned stirring terminates, be down to room temperature, add 30g silane coupling agent wherein, stir, and then add 40g urea wherein, at temperature is 68 DEG C, after stirring 30min, is down to room temperature, composite biomass sizing agent can be obtained.
This example operation is simple, and during use, biomass sizing agent the present invention made is poured into after on spreadometer, and during dry finishing is good, plate is delivered on spreadometer and carried out gluing, and Amount of spread controls at 100g/m
2afterwards plate in glue-coated multilayer is loaded on preformer and carry out precompressed, hot pressing on thermocompressor is put into again after precompressed, arranging hot pressing pressure is 4MPa, and hot pressing temperature is 110 DEG C, takes out after hot pressing 10s, finally sheet material finished product is detected, record free formaldehyde content and be reduced to 1.2% from 7%, clearance, up to 82.8%, reaches the requirement of premium grads.
Example 2
First get 2L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.3, be heated to black liquid boiling, keep temperature 2h, it is even then to add 200mL absolute ethyl alcohol and stirring wherein, filters after leaving standstill 35min; Then by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 200g polyacrylamide wherein and 250mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate; Be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction subsequently, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 200mL dimethyl formamide more wherein to stir, leave standstill after 20min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture; Next the modified lignin resin mixture getting 350g gained puts into container, add 65g starch wherein, mix, then add 165g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 6%, container is placed in water-bath to carry out being heated to 65 DEG C, after stirring 2h, add 180mL vinyl acetate wherein, still aging 8h; After above-mentioned standing end, add 140mL4-tertiary butyl phenol respectively wherein again, 100mL massfraction is the sodium hydroxide solution of 60%, after stirring 35min, add 75mL Myracaldehyde wherein again, be warming up to 85 DEG C, add 80g zinc oxide and carry out catalysis, use nitrogen to protect, stir 2h; Finally after above-mentioned stirring terminates, be down to room temperature, add 55g silane coupling agent wherein, stir, and then add 60g urea wherein, at temperature is 72 DEG C, after stirring 35min, is down to room temperature, composite biomass sizing agent can be obtained.
This example operation is simple, and during use, biomass sizing agent the present invention made is poured into after on spreadometer, and during dry finishing is good, plate is delivered on spreadometer and carried out gluing, and Amount of spread controls at 110g/m
2afterwards plate in glue-coated multilayer is loaded on preformer and carry out precompressed, hot pressing on thermocompressor is put into again after precompressed, arranging hot pressing pressure is 6MPa, and hot pressing temperature is 130 DEG C, takes out after hot pressing 13s, finally sheet material finished product is detected, record free formaldehyde content and be reduced to 1.0% from 6%, clearance, up to 83.3%, reaches the requirement of premium grads.
Example 3
First get 3L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.5, be heated to black liquid boiling, keep temperature 3h, it is even then to add 300mL absolute ethyl alcohol and stirring wherein, filters after leaving standstill 40min; Then by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 300g polyacrylamide wherein and 300mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate; Be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction subsequently, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 230mL dimethyl formamide more wherein to stir, leave standstill after 25min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture; Next the modified lignin resin mixture getting 400g gained puts into container, add 80g starch wherein, mix, then add 150 ~ 180g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 8%, container is placed in water-bath to carry out being heated to 70 DEG C, after stirring 3h, add 200mL vinyl acetate wherein, still aging 10h; After above-mentioned standing end, add 170mL4-tertiary butyl phenol respectively wherein again, 120mL massfraction is the sodium hydroxide solution of 60%, after stirring 40min, add 90mL Myracaldehyde wherein again, be warming up to 90 DEG C, add 100g zinc oxide and carry out catalysis, use nitrogen to protect, stir 3h; Finally after above-mentioned stirring terminates, be down to room temperature, add 60g silane coupling agent wherein, stir, and then add 80g urea wherein, at temperature is 78 DEG C, after stirring 40min, is down to room temperature, composite biomass sizing agent can be obtained.
This example operation is simple, and during use, biomass sizing agent the present invention made is poured into after on spreadometer, and during dry finishing is good, plate is delivered on spreadometer and carried out gluing, and Amount of spread controls at 120g/m
2afterwards plate in glue-coated multilayer is loaded on preformer and carry out precompressed, hot pressing on thermocompressor is put into again after precompressed, arranging hot pressing pressure is 8MPa, and hot pressing temperature is 145 DEG C, takes out after hot pressing 15s, finally sheet material finished product is detected, record free formaldehyde content and be reduced to 0.8% from 5%, clearance, up to 84%, reaches the requirement of premium grads.
Claims (1)
1. utilize black liquid to prepare a method for composite biomass sizing agent, it is characterized in that concrete preparation process is:
(1) get 1 ~ 3L black liquid and put into container, add wherein massfraction be 25% hydrochloric acid soln regulate pH to be 7.0 ~ 7.5, be heated to black liquid boiling, keep temperature 1 ~ 3h, then add 100 ~ 300mL absolute ethyl alcohol and stirring wherein even, filter after leaving standstill 30 ~ 40min;
(2) by the filtered liquid of above-mentioned gained and Glacial acetic acid by volume 3:1 mix, the mixed solution of gained is put into encloses container, add 100 ~ 300g polyacrylamide wherein and 200 ~ 300mL massfraction is the hydrochloric acid soln of 60%, stirring and dissolving, until mix, carbonic acid gas is then used to seal it, the air in amount discharge container, stir until mixture not reflation in container, filter to obtain filtrate;
(3) be the ammoniacal liquor of 30% the filtrate of above-mentioned gained and massfraction, mix by solid-to-liquid ratio 1:3, then container is put in the mixing of gained, add 140 ~ 230mL dimethyl formamide more wherein to stir, leave standstill after 15 ~ 25min, carry out centrifugation, get supernatant liquor and put into spray-drier and carry out spraying dry, collect dry thing, obtain modified lignin resin mixture;
(4) the modified lignin resin mixture getting 300 ~ 400g gained puts into container, add 50 ~ 80g starch wherein, mix, then add 150 ~ 180g ammonium persulphate wherein, functional quality mark is the DMF aqueous solution soaking mixture of 4 ~ 8%, container is placed in water-bath to carry out being heated to 60 ~ 70 DEG C, after stirring 1 ~ 3h, add 150 ~ 200mL vinyl acetate wherein, still aging 5 ~ 10h;
(5) after above-mentioned standing end, 130 ~ 170mL4-tertiary butyl phenol is added respectively wherein, 80 ~ 120mL massfraction is the sodium hydroxide solution of 60%, after stirring 30 ~ 40min, add 60 ~ 90mL Myracaldehyde wherein again, be warming up to 80 ~ 90 DEG C, add 50 ~ 100g zinc oxide and carry out catalysis, use nitrogen to protect, stir 1 ~ 3h;
(6) after above-mentioned stirring terminates, be down to room temperature, add 30 ~ 60g silane coupling agent wherein, stir, and then add 40 ~ 80g urea wherein, at temperature is 68 ~ 78 DEG C, after stirring 30 ~ 40min, be down to room temperature, composite biomass sizing agent can be obtained.
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Cited By (5)
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| CN106085353A (en) * | 2016-06-27 | 2016-11-09 | 高大元 | A kind of preparation method of formaldehydeless lignin-base based Wood Adhesives |
| CN106476367A (en) * | 2016-10-14 | 2017-03-08 | 安徽格义循环经济产业园有限公司 | Lignin phenol formaldehyde resin environment-friendly sheet |
| CN106675058A (en) * | 2016-12-11 | 2017-05-17 | 雷笑天 | Preparation method of biomass graphite electrode bonding agent |
| CN113056503A (en) * | 2018-10-05 | 2021-06-29 | 洛科威国际有限公司 | Method for producing oxidized lignin |
| CN114686121A (en) * | 2020-12-29 | 2022-07-01 | 上海昶法新材料有限公司 | Biomass adhesive and preparation method and application thereof |
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| CN106675058A (en) * | 2016-12-11 | 2017-05-17 | 雷笑天 | Preparation method of biomass graphite electrode bonding agent |
| CN113056503A (en) * | 2018-10-05 | 2021-06-29 | 洛科威国际有限公司 | Method for producing oxidized lignin |
| CN114686121A (en) * | 2020-12-29 | 2022-07-01 | 上海昶法新材料有限公司 | Biomass adhesive and preparation method and application thereof |
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| CN105273666B (en) | 2017-03-08 |
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Effective date of registration: 20161226 Address after: 523059 Guangdong province Dongguan City Wanjiang New Valley Bay community Taixinlu No. 38 Applicant after: Dongguan Sheng Cheng Adhesive Technology Co., Ltd. Address before: Tianhong Technology Building 801 No. 213164 Jiangsu city of Changzhou province Chang Wu Road 416 Applicant before: Lei Chunsheng |
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