CN106317417A - Method for preparing sodium lignin sulfonate with camellia oleifera shells - Google Patents
Method for preparing sodium lignin sulfonate with camellia oleifera shells Download PDFInfo
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- CN106317417A CN106317417A CN201610697405.4A CN201610697405A CN106317417A CN 106317417 A CN106317417 A CN 106317417A CN 201610697405 A CN201610697405 A CN 201610697405A CN 106317417 A CN106317417 A CN 106317417A
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- shell
- weight
- abel
- camelliaoleifera abel
- granule
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Abstract
The invention discloses a method for preparing sodium lignin sulfonate with camellia oleifera shells and relates to the technical field of biological medicine. The method includes the steps of 1), material selecting; 2), soaking; 3), drying; 4), smashing; 5), fermenting; 6), acid splitting; 7), washing; 8), homogenizing; 9), sulfonating; 10), decoloring; 11), concentrating; 12), freezing; 13), drying. The method has the advantages of wide sources of the raw materials, high product purity and the like, and the method is suitable for preparing the sodium lignin sulfonate with the camellia oleifera shells and preparing the sodium lignin sulfonate with agricultural crops of corn sraws, corncobs, sorghum stalks, begasse and the like.
Description
Technical field
The present invention relates to biomedicine technical field, a kind of shell of Camelliaoleifera Abel prepares the method for sodium lignin sulfonate.
Background technology
Sodium lignin sulfonate (sodium ligninsulfonate) is the sodium salt of lignin sulfonic acid, is a kind of natural polymer
Sub-polymer, anionic surfactant, have the strongest dispersibility, is suitable to be dispersed in aqueous medium solid.Due to
Molecular weight and the difference of functional group and there is dispersibility in various degree, can adsorb on the surface of various solid particles, can enter
Row metal ion exchange, also because there is various active group in its organizational structure, thus can produce condensation or and its
His compound generation hydrogen bond action.Industrially, sodium lignin sulfonate is widely used as dispersant and wetting agent.In printing and dyeing industry
Dispersant-the NNO used i.e. compounds with sodium lignin sulfonate for primary raw material.
At present, the preparation method of sodium lignin sulfonate typically has two kinds: one to be to be exchanged through ion by calcium lignosulfonate；
Two is during slurrying, with sodium carbonate or sodium hydroxide, replaces calcium oxide or calcium hydroxide.Additionally, utilize papermaking
The spent pulping liquor of factory is raw material, and general also have three kinds of preparation methoies: one be calcium bisulfite pulp-making method spent pulping liquor in contained
Some sulphite or disulfate hydroxy combining directly and in lignin molecule generate lignosulfonates, and its process is past
Waste liquid adds the lime cream of 10%, at (95 ± 2) DEG C, heats 30min；By calcifying solution standing sedimentation, precipitate leaches, water
Wash after vulcanization acid；Filter, remove calcium sulfate；Then in filtrate, Na is added2CO3, make calcium lignosulfonate change into sodium sulfonate；Instead
Answer temperature to be advisable with 90 DEG C, after reaction 2h, stand, be filtered to remove the impurity such as calcium sulfate；Filtrate concentrates, and crystallisation by cooling obtains product.
Two is with alkali liquor slurrying gained papermaking wastewater as raw material, first adds concentrated sulphuric acid about 50% in waste liquid, stirs 4～6h；So
Afterwards with lime cream, through sedimentation, filtering, making beating, acid is molten, adds sodium carbonate and converts, concentrate, is dried to obtain product.Three is with grass class slurrying
Method gained waste liquid is raw material, and its method is identical with the second.
Disclosed " the residual with preparing alcohol from stress or stalk of agricultural crops of Chinese patent (number of patent application is 201210200672.8)
Thing is the method for raw material production sodium lignin sulfonate ", the method is using the residue of preparing alcohol from stress or stalk of agricultural crops as raw material,
Through techniques such as filtration, evaporation and concentration, sulfonation modifying, spray drying, produce high-quality sodium lignin sulfonate product.
Summary of the invention
It is an object of the invention to provide the preparation side of the sodium lignin sulfonate that a kind of raw material sources are wide, product purity is high
Method.
For achieving the above object, the technical measures that the present invention is taked are that invention one shell of Camelliaoleifera Abel prepares lignin sulfonic acid
The method of sodium, its preparation process is as follows:
(1), get the raw materials ready: select without rotting, without going mouldy, without the fresh shell of Camelliaoleifera Abel of pest and disease damage, standby；
, soak: shell of Camelliaoleifera Abel is put into 2-5 times of weight, volumetric concentration be 75-85% edible ethanol in, normal at room temperature
15-20h is soaked in pressure, filters；Adding 2-4 times of weight, weight concentration again in shell of Camelliaoleifera Abel is the aqueous alkali of 2.5-4.5%,
Pressure be 1.15-1.55MPa, temperature be 50-60 DEG C at process 30-50min, filter, collect soak shell of Camelliaoleifera Abel, standby；
(3), be dried: immersions shell of Camelliaoleifera Abel is transferred in baking oven, 65-70 DEG C, be dried under normal pressure to moisture content less than 8%, must
It is dried shell of Camelliaoleifera Abel, standby；
(4), pulverize: dry shell of Camelliaoleifera Abel is ground into the shell of Camelliaoleifera Abel granule of 5-20 mesh, standby；
(5), fermentation: addition accounts for its weight 25-35% in shell of Camelliaoleifera Abel granule, temperature is the warm water of 35-40 DEG C, adds simultaneously
Enter to account for the leaven of shell of Camelliaoleifera Abel particle weight 8-15.5%, 28-35 DEG C of lower seal fermentation process 1-3 days, then, after fermenting
Shell of Camelliaoleifera Abel granule with clear water wash 1-3 time, obtain ferment oil Camellia oleifera Abel granule, standby；
(6), acidolysis: adding in ferment oil Camellia oleifera Abel granule with crude oil Camellia oleifera Abel granule identical weight, weight concentration is 1.5-
The aqueous acid of 3.0%, stirs evenly, and is heated to 110-140 DEG C by the programming rate of 5-10 DEG C/min, is 1.25-at pressure
Stir process 2.0-3.5h under 2.5MPa；Then, after temperature is down to room temperature naturally, filter, collect acidolysis shell of Camelliaoleifera Abel granule, standby
With；
, washing: by the warm water soaking 30-45min that acidolysis 1-2 times of weight of shell of Camelliaoleifera Abel granule, temperature are 60-70 DEG C,
Filter；Again with the warm water soaking of equivalent weight, the time is 25-30min, filters, must wash shell of Camelliaoleifera Abel granule, standby；
(8), homogenizing: washing shell of Camelliaoleifera Abel granule is dried or dries to moisture less than 10%, more at normal temperatures at homogenizer
Manage into the uniform homogenizing shell of Camelliaoleifera Abel fine particle of more than 200 mesh, standby；
(9), sulfonation: homogenizing shell of Camelliaoleifera Abel granule is put in retort, is simultaneously introduced 1-2 times of weight, temperature is 70-80 DEG C
Warm water, the most continuously stirred 30-50min, make suspension；Then, then add in retort and account for homogenizing oil
1-2 times of weight of Camellia oleifera Abel granule, weight concentration are the sodium sulfite solution of 15-25%, account for homogenizing shell of Camelliaoleifera Abel particle weight 15-
The acetaldehyde of 28%, account for the iron chloride of homogenizing shell of Camelliaoleifera Abel particle weight 3-5%, stir evenly, and press the programming rate heating of 4-8 DEG C/min
To 105-130 DEG C, under in tank, pressure is 0.75-1.5MPa, isothermal holding 2-3.5h；Then, treat that in tank, temperature is down to naturally
After room temperature, filter, collect sulfonating solution, standby；
(10), decolouring: add the decolorising agent accounting for its weight 10-25% in sulfonating solution, then at 40-55 DEG C at stirring
Reason 40-65min, filters, and collects de-inking solution, standby；
(11), concentrate: de-inking solution is 50-60 DEG C in temperature, under conditions of pressure is 1-5KPa, is concentrated into original volume
1/8-1/5, obtains concentrated solution, standby；
(12), freezing: concentrated solution to be transferred in freezer, in concentrated solution, adds the carbonic acid accounting for its weight 10-15% simultaneously
Calcium powder, stirs evenly, quiet 15-28h of putting at 0-6 DEG C, filters, and collects supernatant liquid；Volume it is slowly added to again in supernatant liquid
Concentration is the edible ethanol of more than 90%, makes the volumetric concentration of ethanol in supernatant liquid reach 60-75%, the most quiet puts to without heavy
Precipitation goes out, and filters, and collects precipitation, standby；
(13), it is dried: precipitate with deionized water is dissolved, drying, pulverizing, obtain sodium lignin sulfonate.
Described aqueous alkali is the water-soluble of one or more in sodium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate
Liquid, when for time two or more, weight portion or other ratio such as the ratio of each component is.
Described leaven is cellulase or yeast, it is also possible to be by calcium sulfate: cellulase: yeast is pressed
(0.2-0.35): (4-6): the part by weight of (0.2-1) mixes.
Described sour water is the aqueous solution of one or more in hydrochloric acid, dilute sulfuric acid, oxalic acid, when for time two or more, respectively
The proportioning of component is for waiting weight portion or other ratio.
Described decolorising agent is neutral active charcoal granule or neutral kieselguhr or 100 mesh silica gel, it is also possible to be to be lived by neutrality
Property charcoal granule: neutral kieselguhr: 100 mesh silica gel are by 0.5:(1-1.5): the part by weight of (0.3-0.45) mixes.
The stir speed (S.S.) of described step (6) middle stir process is 15-25r/min.
The stir speed (S.S.) of described step (10) middle stir process is 50-60r/min.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel of the present invention, is to use discarded shell of Camelliaoleifera Abel (that is: camellia oleifera fruit warp
The epidermis shell separated after drying) as raw material, belong to twice laid, thus, its raw material sources are wide.Meanwhile, collection alcohol is devised
Bubble steep with alkali in together with immersion operation, fermentation procedure and hydrolysis procedure and sulfonation operation etc., be stripped of Camellia oleifera Abel cellulose, contracting
The impurity such as aldehyde, the structure of the shell of Camelliaoleifera Abel that loosened, greatly reduce tea saponin, tea albumen, tea polysaccharide equal size, it is to avoid it is to follow-up
The impact of operation so that it is higher that its product goes out rate, therefore prepared product purity is higher.
Table 1 below is the active ingredient detection data of the sodium lignin sulfonate prepared by method of the application present invention:
Table 1 (content of 100g)
| Composition | Content (g) |
| Sodium lignin sulfonate | 97.25 |
| Lignin | 0.24 |
| Polysaccharide | 0.014 |
| Moisture | 1.20 |
From upper table data it can be seen that the sodium lignin sulfonate prepared by method of the application present invention, content is high, quality
Good, it is suitable for the application in each field.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.Description below is in the way of enumerating, but this
Bright protection domain is not limited thereto.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel of the present embodiment, its preparation process is as follows:
(1), get the raw materials ready: select without rotting, without going mouldy, without the fresh shell of Camelliaoleifera Abel of pest and disease damage, standby；
, soak: shell of Camelliaoleifera Abel is put into 4 times of weight, volumetric concentration be 80% edible ethanol in, soak at normal temperatures and pressures
Bubble 18h, filters；Adding 3 times of weight, weight concentrations again in shell of Camelliaoleifera Abel is the sodium hydrate aqueous solution of 3.5%, at pressure is
1.35MPa, temperature are process 40min at 55 DEG C, filter, and collect and soak shell of Camelliaoleifera Abel, standby；
(3), be dried: immersions shell of Camelliaoleifera Abel is transferred in baking oven, 68 DEG C, be dried under normal pressure and be less than 8% to moisture content, obtain dry
Dry shell of Camelliaoleifera Abel, standby；
(4), pulverize: dry shell of Camelliaoleifera Abel is ground into the shell of Camelliaoleifera Abel granule of 15 mesh, standby；
, fermentation: add in shell of Camelliaoleifera Abel granule account for its weight 30%, temperature is the warm water of 38 DEG C, be simultaneously introduced and account for oil
Camellia oleifera Abel particle weight 12%, by calcium sulfate: cellulase: the fermentation that yeast is mixed by the part by weight of 0.3:5:0.7
Agent, 32 DEG C of lower seal fermentation process 2 days, then, washs the shell of Camelliaoleifera Abel granule after fermentation 2 times with clear water, oil tea of must fermenting
Shell granule, standby；
(6), acidolysis: adding in ferment oil Camellia oleifera Abel granule with crude oil Camellia oleifera Abel granule identical weight, weight concentration is 2.5%
Oxalic acid aqueous solution, stir evenly, and be heated to 130 DEG C by the programming rate of 8 DEG C/min, stir process under pressure is 1.8MPa
3h, stir speed (S.S.) is 20r/min；Then, after temperature is down to room temperature naturally, filter, collect acidolysis shell of Camelliaoleifera Abel granule, standby；
(7), washing: by the acidolysis shell of Camelliaoleifera Abel granule warm water soaking 40min that 2 times of weight, temperature are 65 DEG C, filter；Use again
The warm water soaking of equivalent weight, the time is 28min, filters, must wash shell of Camelliaoleifera Abel granule, standby；
(8), homogenizing: washing shell of Camelliaoleifera Abel granule is dried or dries to moisture less than 10%, more at normal temperatures at homogenizer
Manage into the uniform homogenizing shell of Camelliaoleifera Abel fine particle of more than 200 mesh, standby；
(9), sulfonation: homogenizing shell of Camelliaoleifera Abel granule is put in retort, is simultaneously introduced 1-2 times of weight, temperature is 70-80 DEG C
Warm water, the most continuously stirred 30-50min, make suspension；Then, then add in retort and account for homogenizing oil
2 times of weight of Camellia oleifera Abel granule, weight concentration are the sodium sulfite solution of 20%, account for the second of homogenizing shell of Camelliaoleifera Abel particle weight 22%
Aldehyde, account for the iron chloride of homogenizing shell of Camelliaoleifera Abel particle weight 4%, stir evenly, and be heated to 120 DEG C by the programming rate of 6 DEG C/min, at tank
Middle pressure is under 1MPa, isothermal holding 3h；Then, after temperature is down to room temperature naturally in tank, filter, collect sulfonating solution, standby
With；
(10), decolouring: add in sulfonating solution and account for its weight 18%, by neutral active charcoal granule: neutral kieselguhr: 100
The decolorising agent that mesh silica gel is mixed by the part by weight of 0.5:1.2:0.4, then stir process 55min at 50 DEG C, stirring
Speed is 55r/min, filters, and collects de-inking solution, standby；
(11), concentrate: de-inking solution is 55 DEG C in temperature, under conditions of pressure is 3KPa, is concentrated into the 1/6 of original volume,
Obtain concentrated solution, standby；
(12), freezing: concentrated solution to be transferred in freezer, in concentrated solution, adds the Paris white accounting for its weight 12% simultaneously
End, stirs evenly, quiet 22h of putting at 3 DEG C, filters, and collects supernatant liquid；Being slowly added to volumetric concentration again in supernatant liquid is 90%
Above edible ethanol, makes the volumetric concentration of ethanol in supernatant liquid reach 65%, the most quiet puts to without Precipitation, filters,
Collect precipitation, standby；
(13), it is dried: precipitate with deionized water is dissolved, drying, pulverizing, obtain sodium lignin sulfonate.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel of the present invention, is suitable for preparing lignin sulfonic acid with shell of Camelliaoleifera Abel
Sodium is it can also be used to prepare sodium lignin sulfonate with agricultural crops garbages such as corn stalk, corn cob, Sorghum vulgare Pers. straw stalk, bagasse.
Claims (7)
1. the method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel, it is characterised in that preparation process is as follows:
(1), get the raw materials ready: select without rotting, without going mouldy, without the fresh shell of Camelliaoleifera Abel of pest and disease damage, standby；
, soak: shell of Camelliaoleifera Abel is put into 2-5 times of weight, volumetric concentration be 75-85% edible ethanol in, at normal temperatures and pressures
Soak 15-20h, filter；Adding 2-4 times of weight, weight concentration again in shell of Camelliaoleifera Abel is the aqueous alkali of 2.5-4.5%, in pressure
Power is 1.15-1.55MPa, temperature processes 30-50min at being 50-60 DEG C, filters, and collects and soaks shell of Camelliaoleifera Abel, standby；
(3), be dried: immersions shell of Camelliaoleifera Abel is transferred in baking oven, 65-70 DEG C, be dried under normal pressure and be less than 8% to moisture content, obtain dry
Shell of Camelliaoleifera Abel, standby；
(4), pulverize: dry shell of Camelliaoleifera Abel is ground into the shell of Camelliaoleifera Abel granule of 5-20 mesh, standby；
(5), fermentation: addition accounts for its weight 25-35% in shell of Camelliaoleifera Abel granule, temperature is the warm water of 35-40 DEG C, is simultaneously introduced and accounts for
The leaven of shell of Camelliaoleifera Abel particle weight 8-15.5%, 28-35 DEG C of lower seal fermentation process 1-3 days, then, by the oil after fermentation
Camellia oleifera Abel granule clear water washs 1-3 time, obtains ferment oil Camellia oleifera Abel granule, standby；
(6), acidolysis: adding in ferment oil Camellia oleifera Abel granule with crude oil Camellia oleifera Abel granule identical weight, weight concentration is 1.5-3.0%
Aqueous acid, stir evenly, and be heated to 110-140 DEG C by the programming rate of 5-10 DEG C/min, under pressure is 1.25-2.5MPa
Stir process 2.0-3.5h；Then, after temperature is down to room temperature naturally, filter, collect acidolysis shell of Camelliaoleifera Abel granule, standby；
(7), washing: by the warm water soaking 30-45min that acidolysis 1-2 times of weight of shell of Camelliaoleifera Abel granule, temperature are 60-70 DEG C, filter；
Again with the warm water soaking of equivalent weight, the time is 25-30min, filters, must wash shell of Camelliaoleifera Abel granule, standby；
(8), homogenizing: washing shell of Camelliaoleifera Abel granule dried or dries to moisture less than 10%, then being processed into through homogenizer at normal temperatures
It is more than 200 mesh that uniform homogenizing shell of Camelliaoleifera Abel fine particle, standby；
(9), sulfonation: homogenizing shell of Camelliaoleifera Abel granule is put in retort, is simultaneously introduced 1-2 times of weight, temperature is the temperature of 70-80 DEG C
Water, the most continuously stirred 30-50min, makes suspension；Then, then add in retort and account for homogenizing shell of Camelliaoleifera Abel
1-2 times of weight of granule, weight concentration are the sodium sulfite solution of 15-25%, account for homogenizing shell of Camelliaoleifera Abel particle weight 15-28%
Acetaldehyde, account for the iron chloride of homogenizing shell of Camelliaoleifera Abel particle weight 3-5%, stir evenly, and be heated to 105-by the programming rate of 4-8 DEG C/min
130 DEG C, under in tank, pressure is 0.75-1.5MPa, isothermal holding 2-3.5h；Then, after in tank, temperature is down to room temperature naturally,
Filter, collect sulfonating solution, standby；
(10), decolouring: add the decolorising agent accounting for its weight 10-25%, then stir process at 40-55 DEG C in sulfonating solution
40-65min, filters, and collects de-inking solution, standby；
(11), concentrate: de-inking solution is 50-60 DEG C in temperature, under conditions of pressure is 1-5KPa, is concentrated into the 1/8-of original volume
1/5, obtain concentrated solution, standby；
(12), freezing: concentrated solution to be transferred in freezer, in concentrated solution, adds the Paris white accounting for its weight 10-15% simultaneously
End, stirs evenly, quiet 15-28h of putting at 0-6 DEG C, filters, and collects supernatant liquid；Volumetric concentration it is slowly added to again in supernatant liquid
Being the edible ethanol of more than 90%, make the volumetric concentration of ethanol in supernatant liquid reach 60-75%, the most quiet putting is analysed to without precipitation
Go out, filter, collect precipitation, standby；
(13), it is dried: precipitate with deionized water is dissolved, drying, pulverizing, obtain sodium lignin sulfonate.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described aqueous alkali is molten
Liquid is the aqueous solution of one or more in sodium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate, when for time two or more, respectively
The proportioning of component is for waiting weight portion or other ratio.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described leaven
It is by calcium sulfate: cellulase: yeast presses (0.2-0.35): (4-6): the part by weight of (0.2-1) mixes.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described sour water is
The aqueous solution of one or more in hydrochloric acid, dilute sulfuric acid, oxalic acid, when for time two or more, the weight portion such as the ratio of each component is
Or other ratio.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described decolorising agent
It is by neutral active charcoal granule: neutral kieselguhr: 100 mesh silica gel are by 0.5:(1-1.5): the part by weight mixing of (0.3-0.45)
Form.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described step (6) in
The stir speed (S.S.) of stir process is 15-25r/min.
The method preparing sodium lignin sulfonate with shell of Camelliaoleifera Abel the most according to claim 1, it is characterised in that: described step (10) in
The stir speed (S.S.) of stir process is 50-60r/min.
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Cited By (1)
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| CN109592802A (en) * | 2017-09-30 | 2019-04-09 | 张忠诚 | A kind of multifunctional bio pharmacy water treatment agent and preparation method thereof for water process |
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Application publication date: 20170111 |