CN108455713B - Waste paper deinking wastewater flocculant and preparation method thereof - Google Patents

Waste paper deinking wastewater flocculant and preparation method thereof Download PDF

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CN108455713B
CN108455713B CN201810223441.6A CN201810223441A CN108455713B CN 108455713 B CN108455713 B CN 108455713B CN 201810223441 A CN201810223441 A CN 201810223441A CN 108455713 B CN108455713 B CN 108455713B
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parts
lignin
water
waste paper
temperature
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CN108455713A (en
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杨仁春
林琪童
朱全中
马冠
耿烨松
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Nanyang Zhonghao Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/26Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
    • C02F2103/28Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
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Abstract

The invention discloses a waste paper deinking wastewater flocculant and a preparation method thereof, wherein the waste paper deinking wastewater flocculant is prepared from the following raw materials: organic polymer material, calcium chloride, ferric chloride, aluminum hydroxide, ferric hydroxide and water. The waste paper deinking wastewater flocculant and the preparation method thereof have simple process, can well control the product cost, have the advantages of good treatment effect, obviously improved treatment speed, low wastewater treatment cost and the like, thereby improving the utilization rate of water resources, having strong adsorption and flocculation effects on ink pigment particles, soluble pigments, dyes and the like, being biodegradable and environment-friendly, and leading the adsorbed wastewater to reach the reclaimed water reuse standard.

Description

Waste paper deinking wastewater flocculant and preparation method thereof
Technical Field
The invention relates to the technical field of water treatment agents, and particularly relates to a waste paper deinking wastewater flocculant and a preparation method thereof.
Background
In recent years, the output and sales of the paper industry in China are steadily increased, so that the demand of paper making raw materials is continuously increased, the paper making raw materials in China, particularly wood raw materials, are lacked, and the recovery and utilization of waste paper become important raw materials supporting the development of the paper industry in China. In 2011, the consumption of waste paper in China is 5660 ten thousand tons, which accounts for 62.58 percent of the total consumption of paper pulp. Wherein more than 20 percent of waste paper is old magazine paper, old newspaper and mixed waste paper, and needs deinking in the production process, and the deinking mainly comprises the following steps: (1) the waste paper is broken under alkaline condition to separate the printing ink from the fiber; (2) the ink is floated in a flotation tank. The conventional deinking process is to add fatty acid and calcium chloride, and the formed calcium soap promotes the aggregation of carbon black particles, so that the carbon black particles are attached to bubbles and floated. Part of the ink is separated and treated in the form of solid waste, and part of the ink remains in the deinking waste water.
The waste paper is utilized for pulping and papermaking, the waste water mainly comes from deinking, pulping, pulp purification and screening of the waste paper and a wet part of a paper machine, the waste water amount is very large, 1 ton of deinked pulp is generally produced singly, the waste water amount is higher than 100 tons, and if the waste water generated by the pulping, the purification and the wet part of the paper machine is added, the waste water amount is larger; and the pollution indexes such as printing ink, SS (suspended solid), COD (chemical oxygen demand) and BOD (biochemical oxygen demand) in the wastewater are high, the pollution indexes greatly exceed the discharge standard of the paper industry wastewater regulated by the state, and when the BOD/COD in the deinking wastewater is less than 30%, the biochemical treatment performance of the deinking wastewater is poor, so that the deinking wastewater belongs to the industrial wastewater which is difficult to treat, and how to reasonably treat the wastewater is a great problem for environmental engineering workers.
In the water treatment process, the flocculant mainly neutralizes the groups with positive (negative) electric property and some particles with negative (positive) electric property which are difficult to separate in water, lowers the electric potential, makes the particles in an unstable state, and uses the polymerization property to make the particles gather and be separated by a physical or chemical method. The flocculating agent mainly comprises inorganic and organic substances. The inorganic flocculant is cheap, the organic polymer flocculant is small in dosage, the scum yield is low, the flocculation capacity is strong, the floc is easy to separate, and the oil removal and suspended matter removal effects are good.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a waste paper deinking wastewater flocculant and a preparation method thereof.
The technical scheme of the invention is as follows:
a waste paper deinking wastewater flocculant is prepared from the following raw materials: organic polymer material, calcium chloride, ferric chloride, aluminum hydroxide, ferric hydroxide and water.
A waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 95-105 parts of organic polymer material, 5-15 parts of calcium chloride, 5-15 parts of ferric chloride, 15-25 parts of aluminum hydroxide, 10-20 parts of ferric hydroxide and 550 parts of water.
The organic polymer material is lignin.
Further, the organic polymer material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at the water vapor pressure of 0.3-1.3MPa and the temperature of 150-; soaking lignin in gallic acid water solution for 15-25min, filtering, and drying to obtain lignin after soaking treatment; adding 95-105g of lignin subjected to the dipping treatment into 290-310g of water, then adding 15-25g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 20-40 ℃ for 30-60 min; adding 15-25g of sodium chloroacetate and 25-35g of quaternary ammonium salt, reacting at 60-80 ℃ for 1.5-3.5h, filtering, washing the obtained filter residue with water, and drying to obtain the product.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 35-45%.
The drying temperature is 60-80 ℃ and the drying time is 15-25 h.
The mass fraction of gallic acid in the gallic acid aqueous solution is 6-12%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: (2-5).
The quaternary ammonium salt is 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride and/or (3-acrylamide propyl) trimethyl ammonium chloride. In one embodiment of the present invention, the quaternary ammonium salt consists of 60-70 wt% of 3-abietylamino-2-hydroxypropyltrimethylammonium chloride and 30-40 wt% (3-acrylamidopropyl) trimethylammonium chloride.
The invention also provides a preparation method of the waste paper deinking wastewater flocculant, which comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 3-5h at the temperature of 140-.
The technical effects are as follows:
the waste paper deinking wastewater flocculant and the preparation method thereof have simple process, can well control the product cost, have the advantages of good treatment effect, obviously improved treatment speed, low wastewater treatment cost and the like, thereby improving the utilization rate of water resources, having strong adsorption and flocculation effects on ink pigment particles, soluble pigments, dyes and the like, being biodegradable and environment-friendly, and leading the adsorbed wastewater to reach the reclaimed water reuse standard.
Detailed Description
And (3) determination of degerming performance: inoculating strain of Staphylococcus aureus (Staphylococcus aureus) AS.1.89, inoculating to nutrient broth, culturing at 37 deg.C for 24 hr, and diluting with sterile physiological saline to cell concentration of 104CFU/mL of initial broth. Taking 0.1g of waste paper deinking wastewater flocculant into a sterilized conical flask, sucking 1.0mL of initial bacterial liquid by using a sterilized scale suction pipe, slowly and uniformly dripping the initial bacterial liquid on an environment-friendly water treatment agent, and sealing a bottle mouth. Adding 50mL of sterilized normal saline into a bottle after 1h, violently shaking for 2min, settling for 30min, filtering with a 0.45-micrometer filter membrane, and taking an appropriate amount of solution to determine the total number of bacteria by a gradient dilution method; and a blank control of the environment-friendly water treatment agent without the bacteriostatic agent is made. The experimental results are the average of three experiments. The bacteria removal rate (%) × (1-total number of bacteria in experimental group/total number of bacteria in control group) × 100%.
Removal of Cr6+Experiment: weighing 1g of waste paper deinking wastewater flocculant, adding the flocculant into a 150mL iodine flask, and then adding Cr6+100mL of an aqueous solution having an initial concentration of 350mg/L, tightly covering and sealing with a sealing film, oscillating at a constant temperature of 150 rpm at 25 ℃ to equilibrate, settling for 30min, filtering with a 0.45 μm filter, measuring Cr before and after adsorption6+The concentration change of Cr is calculated by the following formula6+The removal rate is as follows: cr (chromium) component6+Removal rate ═ C0-C)/C0In which C is0Is Cr in solution before adsorption6+C is Cr in the adsorbed solution6+(iii) concentration (mg/L). Cr (chromium) component6+The determination of (1):flame atomic absorption spectrophotometry, with a measurement wavelength of 357.9 nm.
Ink removal experiments: weighing 1g of waste paper deinking wastewater flocculant, adding the flocculant into a 150mL iodine bottle, adding 100mL of aqueous solution with the initial concentration of ink of 400mg/L, wherein the ink is GV6134 black environment-friendly surface printing ink provided by Guangdong cis-German special chemical company, covering tightly, sealing by using a sealing film, oscillating at a constant temperature of 150 rpm at 25 ℃ to balance, filtering by using a 0.45-micron filter membrane after settling for 30min, measuring the concentration change of the ink before and after adsorption, and calculating the removal rate of the ink according to the following formula: ink removal rate ═ C3-C4)/C3In which C is3Is the concentration of ink in the solution before adsorption (mg/L), C4The concentration of the ink in the solution after adsorption (mg/L) was used. Measurement of ink concentration: the method is carried out according to the method shown in example 1 in Chinese patent application No. 201310259929.1.
Introduction of raw materials in the examples:
(3-acrylamidopropyl) trimethylammonium chloride, CAS No.: 45021-77-0.
Calcium chloride, CAS number: 14336-71-1.
Ferric chloride, CAS No.: 7705-08-0.
Aluminum hydroxide, CAS No.: 21645-51-2.
Iron hydroxide, CAS No.: 1309-33-7.
Gallic acid, CAS No.: 149-91-7.
Sodium hydroxide, CAS No.: 1310-73-2.
Sodium chloroacetate, CAS No.: 3926-62-3.
3-rosin amino-2-hydroxypropyl trimethyl ammonium chloride was prepared according to the synthesis conditions and methods identified in the paper "synthesis research of 3-rosin amino-2-hydroxypropyl trimethyl ammonium chloride" published by vermilion, cai zhen, yang chun, and shangshen, and the synthesis conditions were as follows: ethanol as reaction medium, solid-carried potassium carbonate (potassium carbonate content is 20%) as catalyst and acid-binding agent, and nK2CO3The reaction time is 12h, wherein RA is abietylamine and CTA is 3-chloro-2-hydroxypropyl trimethyl ammonium chloride.
The lignin is high-purity lignin provided by environmental protection materials of the Jinhai of Jinan, and the product grade is a superior product.
Example 1
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of lignin, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 2
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and then adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting for 2.5h at the temperature of 70 ℃ and the rotating speed of 90r/min, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue by using 200g of water, and drying for 20h at the temperature of 75 ℃ to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The mass fraction of gallic acid in the gallic acid aqueous solution is 8%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3.
the quaternary ammonium salt is 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 3
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; adding 100g of lignin subjected to steam infiltration treatment into 300g of water, adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and then adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting for 2.5h at the temperature of 70 ℃ and the rotating speed of 90r/min, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue by using 200g of water, and drying for 20h at the temperature of 75 ℃ to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The quaternary ammonium salt is 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 4
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin after soaking treatment; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and then adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting for 2.5h at the temperature of 70 ℃ and the rotating speed of 90r/min, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue by using 200g of water, and drying for 20h at the temperature of 75 ℃ to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The mass fraction of gallic acid in the gallic acid aqueous solution is 8%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3.
the quaternary ammonium salt is 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 5
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and then adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting for 2.5h at the temperature of 70 ℃ and the rotating speed of 90r/min, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue by using 200g of water, and drying for 20h at the temperature of 75 ℃ to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The mass fraction of gallic acid in the gallic acid aqueous solution is 8%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3.
the quaternary ammonium salt is (3-acrylamide propyl) trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 6
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and adding 20g of sodium chloroacetate, reacting at 70 ℃ at a rotating speed of 90r/min for 2.5h, filtering by using 500-mesh filter cloth, washing the obtained filter residue with 200g of water, and drying at 75 ℃ for 20h to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The mass fraction of gallic acid in the gallic acid aqueous solution is 8%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3.
the quaternary ammonium salt is 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
Example 7
The waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water.
The organic high molecular material is pretreated lignin.
The preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; and then adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting for 2.5h at the temperature of 70 ℃ and the rotating speed of 90r/min, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue by using 200g of water, and drying for 20h at the temperature of 75 ℃ to obtain the pretreated lignin.
The mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40%.
The mass fraction of gallic acid in the gallic acid aqueous solution is 8%.
The mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3.
the quaternary ammonium salt is formed by mixing 65 wt% of 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride and 35 wt% of (3-acrylamide propyl) trimethyl ammonium chloride.
The preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant. The performance test result of the waste paper deinking wastewater flocculant is as follows: cr (chromium) component6+The removal rate was 94%, the ink removal rate was 91%, and the sterilization rate was 98%.
Test example 1
The performance test of the waste paper deinking wastewater flocculant prepared in the examples 2 to 6 is carried out, and the specific test results are shown in the table 1.
Table 1: test result table
Figure BDA0001600603210000091
Figure BDA0001600603210000101
The waste paper deinking wastewater flocculant prepared by a large number of researches has strong adsorption flocculation effect on ink pigment particles, soluble pigment, dye and the like, is biodegradable and environment-friendly, and the adsorbed wastewater reaches the reclaimed water reuse standard.

Claims (6)

1. The waste paper deinking wastewater flocculant is characterized by being prepared from the following raw materials in parts by weight: 95-105 parts of organic polymer material, 5-15 parts of calcium chloride, 5-15 parts of ferric chloride, 15-25 parts of aluminum hydroxide, 10-20 parts of ferric hydroxide and 550 parts of water;
the organic high polymer material is pretreated lignin;
the preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at the water vapor pressure of 0.3-1.3MPa and the temperature of 150-; soaking lignin in gallic acid water solution for 15-25min, filtering, and drying to obtain lignin after soaking treatment; adding 95-105g of lignin subjected to the dipping treatment into 290-310g of water, then adding 15-25g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 20-40 ℃ for 30-60 min; adding 15-25g of sodium chloroacetate and 25-35g of quaternary ammonium salt, reacting at 60-80 ℃ for 1.5-3.5h, filtering, washing the obtained filter residue with water, and drying to obtain the product;
the quaternary ammonium salt consists of 60-70 wt% of 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride and 30-40 wt% of (3-acrylamide propyl) trimethyl ammonium chloride.
2. The waste paper deinking wastewater flocculant according to claim 1, wherein the mass fraction of sodium hydroxide in the aqueous sodium hydroxide solution is from 35 to 45%, and the mass fraction of gallic acid in the aqueous gallic acid solution is from 6 to 12%.
3. The waste paper deinking waste water flocculant of claim 1, wherein said drying is carried out at a temperature of 60 to 80 ℃ for 15 to 25 hours.
4. The waste paper deinking wastewater flocculant according to claim 1, wherein the mass ratio of the lignin after the steam-moistening treatment to the aqueous solution of gallic acid is 1: (2-5).
5. The process for producing a flocculant for waste paper deinking waste water according to any one of claims 1 to 4, characterized by comprising the steps of:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 3-5h at the temperature of 140-.
6. The waste paper deinking waste water flocculant of claim 1,
the waste paper deinking wastewater flocculant is prepared from the following raw materials in parts by weight: 100 parts of organic polymer material, 10 parts of calcium chloride, 10 parts of ferric chloride, 20 parts of aluminum hydroxide, 15 parts of ferric hydroxide and 500 parts of water;
the organic high polymer material is pretreated lignin;
the preparation method of the pretreated lignin comprises the following steps: performing steam infiltration treatment on lignin at water vapor pressure of 1MPa and temperature of 180 deg.C for 10 min; soaking lignin in gallic acid water solution for 20min, filtering with 500 mesh filter cloth, and drying at 75 deg.C for 20 hr to obtain lignin; adding 100g of the lignin subjected to the dipping treatment into 300g of water, then adding 20g of sodium hydroxide aqueous solution, and stirring and reacting at the temperature of 30 ℃ and the rotating speed of 90r/min for 50 min; adding 20g of sodium chloroacetate and 30g of quaternary ammonium salt, reacting at 70 ℃ at a rotating speed of 90r/min for 2.5h, filtering by adopting 500-mesh filter cloth, washing the obtained filter residue with 200g of water, and drying at 75 ℃ for 20h to obtain the pretreated lignin;
the mass fraction of sodium hydroxide in the sodium hydroxide aqueous solution is 40 percent;
the mass fraction of gallic acid in the gallic acid aqueous solution is 8%;
the mass ratio of the lignin subjected to steam infiltration treatment to the gallic acid aqueous solution is 1: 3;
the quaternary ammonium salt is formed by mixing 65 wt% of 3-abietylamine-2-hydroxypropyl trimethyl ammonium chloride and 35 wt% of (3-acrylamide propyl) trimethyl ammonium chloride;
the preparation method of the waste paper deinking wastewater flocculant comprises the following steps:
(1) weighing the raw materials in parts by weight;
(2) adding the raw materials into a high-pressure reaction kettle, stirring and reacting for 4 hours at the temperature of 150 ℃ and the pressure of 0.4MPa at the rotating speed of 90r/min, cooling to room temperature, filtering by adopting 500-mesh filter cloth, and drying filter cakes for 15 hours at the temperature of 120 ℃ to obtain the waste paper deinking wastewater flocculant.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011022644A2 (en) * 2009-08-21 2011-02-24 Auburn University Fermentation and chemical treatment of pulp and paper mill sludge
WO2011162420A1 (en) * 2010-06-25 2011-12-29 ロペスアンドエヌティ有限会社 Method for recovering lignin in the neutral range from spent pulp cooking liquor
CN102992458A (en) * 2012-11-26 2013-03-27 洪仁作 Flocculating agent for treating leather waste water
CN104229957A (en) * 2013-06-24 2014-12-24 张家领 Compound flocculant taking natural minerals as main components
CN105314722A (en) * 2015-11-12 2016-02-10 合肥安奎思成套设备有限公司 Efficient sewage treatment flocculant and preparation method thereof
CN105384231A (en) * 2015-12-22 2016-03-09 山东大学 Polyaluminum ferric chloride-paper mill sludge based polymer composite flocculant and preparation method thereof
CA2974783A1 (en) * 2015-01-28 2016-09-15 Weteq S.A. Combination of flocculant with surfactant for wastewater treatment

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9776900B2 (en) * 2014-01-14 2017-10-03 Buckman Laboratories International, Inc. Use of celluloses in sludge dewatering, and sludge products thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011022644A2 (en) * 2009-08-21 2011-02-24 Auburn University Fermentation and chemical treatment of pulp and paper mill sludge
WO2011162420A1 (en) * 2010-06-25 2011-12-29 ロペスアンドエヌティ有限会社 Method for recovering lignin in the neutral range from spent pulp cooking liquor
CN102992458A (en) * 2012-11-26 2013-03-27 洪仁作 Flocculating agent for treating leather waste water
CN104229957A (en) * 2013-06-24 2014-12-24 张家领 Compound flocculant taking natural minerals as main components
CA2974783A1 (en) * 2015-01-28 2016-09-15 Weteq S.A. Combination of flocculant with surfactant for wastewater treatment
CN105314722A (en) * 2015-11-12 2016-02-10 合肥安奎思成套设备有限公司 Efficient sewage treatment flocculant and preparation method thereof
CN105384231A (en) * 2015-12-22 2016-03-09 山东大学 Polyaluminum ferric chloride-paper mill sludge based polymer composite flocculant and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
新型脱色絮凝剂木素季胺盐的研制及其絮凝性能与机理的研究;吴冰艳等;《化工环保》;19971030(第5期);第12-16页 *
木质素基脱色絮凝剂深度处理制浆造纸废水;乔瑞平等;《化学工程》;20090915;第37卷(第09期);第48-51页 *
木质素磺酸钠络合能力的影响因素及其改性研究;冯雪敏;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20151225(第12期);第14页 *

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