AU2020244447B2 - Method for preparing efficient dyeing wastewater adsorbent from waste goat hair - Google Patents
Method for preparing efficient dyeing wastewater adsorbent from waste goat hair Download PDFInfo
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- 241000283707 Capra Species 0.000 title claims abstract description 167
- 210000004209 hair Anatomy 0.000 title claims abstract description 159
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002699 waste material Substances 0.000 title claims abstract description 34
- 239000003463 adsorbent Substances 0.000 title claims abstract description 31
- 239000002351 wastewater Substances 0.000 title claims abstract description 27
- 238000004043 dyeing Methods 0.000 title claims abstract description 23
- 238000001179 sorption measurement Methods 0.000 claims abstract description 68
- 238000004880 explosion Methods 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000007710 freezing Methods 0.000 claims abstract description 22
- 230000008014 freezing Effects 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000000985 reactive dye Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 238000011282 treatment Methods 0.000 abstract description 28
- 239000000975 dye Substances 0.000 abstract description 17
- 239000013078 crystal Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000002203 pretreatment Methods 0.000 abstract description 3
- 238000002336 sorption--desorption measurement Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 239000011148 porous material Substances 0.000 description 17
- 230000001186 cumulative effect Effects 0.000 description 10
- 210000002268 wool Anatomy 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000006872 improvement Effects 0.000 description 5
- 102000011782 Keratins Human genes 0.000 description 4
- 108010076876 Keratins Proteins 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000000295 complement effect Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 241000287828 Gallus gallus Species 0.000 description 2
- 210000000085 cashmere Anatomy 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 210000003746 feather Anatomy 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 240000001548 Camellia japonica Species 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000011511 Diospyros Nutrition 0.000 description 1
- 244000236655 Diospyros kaki Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000002159 adsorption--desorption isotherm Methods 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000018597 common camellia Nutrition 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Substances OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- KUIXZSYWBHSYCN-UHFFFAOYSA-L remazol brilliant blue r Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C(N)=C2C(=O)C3=CC=CC=C3C(=O)C2=C1NC1=CC=CC(S(=O)(=O)CCOS([O-])(=O)=O)=C1 KUIXZSYWBHSYCN-UHFFFAOYSA-L 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4856—Proteins, DNA
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
Disclosed is a method for preparing an efficient dyeing wastewater adsorbent from waste goat
hair, which belongs to the field of bio-based adsorption materials. Steam explosion and
disintegration with the liquid nitrogen freezing disintegrator are combined to treat the waste
goat hair. The steam explosion and disintegration with the liquid nitrogen freezing disintegrator
technology used in the present invention is an efficient and environment-friendly pretreatment
method. In addition, after the treatment, the goat hair powder has particles of as low as 20 Im,
and a crystal index of as low as 2.6%, which increases an amorphous region of the goat hair
powder, thereby facilitating the absorption effect of the goat hair. The goat hair adsorbent
prepared by the method of the present invention absorbs dyes in dyeing wastewater, with a
dye removal rate up to 95%, and an adsorption capacity up to 426 mg/g, which is an excellent
biological adsorbent; the goat hair adsorbent prepared by the method of the present invention
can repeat adsorption-desorption cycles 5 to 6 times.
Description
Method for Preparing Efficient Dyeing Wastewater Adsorbent from Waste Goat
Hair
Technical Field
[0001] The present invention relates to a method for preparing an efficient dyeing wastewater
adsorbent from waste goat hair, which belongs to the field of bio-based adsorption materials.
Background
[0002] According to statistics, there are 1.074 billion goats globally, which are fed mainly in
China, Mongolia, and Iran. Goats can provide two kinds of fibers, goat hair and cashmere
respectively. Cashmere is one kind of rare animal fibers and is commonly called as "soft gold"
and "gem in fiber". However, its waste goat hair is non-curly, rough and hard, and has low
utilization value. At present, the method of reducing agent-formic acid is mainly used to
prepare goat hair keratin solution. Due to secondary pollution and high cost, these have not
been actually used. Therefore, further research on the application of goat hair is needed.
[0003] Textile dyeing industry leads to a large amount of wastewater. The annual consumption
of dyes in the world exceeds 70,000 tons, of which 45% are reactive dyes. Reactive dyes can be
used to dye cellulose fibers such as cotton and viscose. A large amount of reactive dyes is not
fixed on the cellulose fibers and enter the water to form reactive dye wastewater. Therefore,
the treatment of reactive dye wastewater has become an important issue. Reactive dye 19 (RB
19) is widely used in textile dyeing and is a non-biodegradable pollutant, so it is commonly used
as a model dye in many studies.
[0004] In biological treatment, flocculation, membrane separation processes, chemical
precipitation, adsorption (using activated carbon) and ion exchange and other dyeing
wastewater treatment methods, adsorption has been proven to be an economical and effective
method. With the strengthening of people's awareness of environmental protection, people have put forward higher requirements for adsorbents for treating dye wastewater, requiring environmental protection, low cost, good adsorption performance and reusable.
[0005] The use of agricultural waste as unconventional adsorbents to treat dye wastewater has
become an important topic at present, such as chitosan, polyethyleneimine cationic modified
persimmon tannin adsorbent, wheat straw, coconut leaves, corncob-xylose-based residue
adsorbent, camellia nut shell, fruit peel, etc. Goat wool has a large number of active groups
such as amino and carboxyl groups, which can be used as an adsorbent. While, the problem is
that the amount of adsorption is small. In order to solve this problem, it appears in the
literature that chicken feathers are used as raw materials to extract keratin and then prepare
sponge absorbents, however, the cost is high. Someone proposed to use hair as the raw
material, and after pretreatment with NaOH aqueous solution, it was modified with
formaldehyde and dimethylamine in two steps to prepare a modified keratin adsorbent
containing quaternary ammonium salt. However, the modification method is complicated and
not environmentally friendly.
[0006] The research showed that the extracted keratin from chicken feathers had good
adsorption properties (Song et al., 2017).
Summary
[0007] In an attempt to improve the utilization rate of waste goat hair resources and provide a
low-cost green adsorbent for the treatment of reactive dye wastewater, the present invention
adopts an efficient, environment-friendly and fast pretreatment method, i.e. a steam explosion
method, to perform steam explosion pretreatment on the waste goat hair. After the goat hair is
steam exploded and liquid nitrogen disintegrated, powder with a particle size of 10 to 30 um (in
some embodiments, 15 to 30 um) is obtained, which can be used as a dyeing wastewater
biological adsorbent for treating reactive dye wastewater. The adsorption capacity to reactive dyes is increased from 55 mg/g to 426 mg/g, which increases by about 7 times; and meanwhile, it is ensured that the yield of the goat hair after being steam exploded is 85% or above.
[0008] The present invention discloses a method for preparing an efficient dyeing wastewater
adsorbent from waste goat hair, which adopts steam explosion and disintegration with the
liquid nitrogen freezing disintegrator to treat the waste goat hair.
[0008a] In an embodiment of the present invention, steam explosion conditions are: an
explosion pressure of 1.3 MPa to 1.7 MPa, and an explosion time of 30 s to 240 s.
[0008b] In an embodiment of the present invention, the method comprises the following steps:
(1) steam explosion: performing steam explosion on the waste goat hair, and freeze-drying; and
(2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid nitrogen
freezing disintegrator on the goat hair in step (1) to obtain the goat hair powder.
[0009] In an embodiment of the present invention, the method comprises the following steps:
[0010] (1) steam explosion: performing steam explosion on the waste goat hair, sieving with a
200 to 300 mesh sieve, and then freeze-drying; and
[0011] (2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid
nitrogen freezing disintegrator on the goat hair in step (1) to obtain goat hair powder with a
particle size of 10 to 30 Iim.
[0012] Paragraph [0012] is intentionally deleted.
[0013] In an embodiment of the present invention, the freeze-drying in step (1) is to place the
steam-exploded sample at -60 to -80°C for freezing for 1 to 4 h, and then dry the goat hair by
using vacuum freeze-drying.
[0014] In an embodiment of the present invention, vacuum freeze-drying conditions are: a
vacuum degree of 5 to 15 Pa, a temperature of -40 to -60°C, and a drying time of 36 to 72 h.
[0014a] In an embodiment of the present invention, the method comprises the following steps:
(1) steam explosion: performing steam explosion on the waste goat hair, wherein a steam
explosion pressure is 1.5 MPa, and a steam explosion time is 150 s; filtering to remove water in
the steam-exploded goat hair with a 200 mesh screen; placing the steam-exploded sample in an
ultra-low temperature refrigerator at -80°C for 2 h, and then drying the goat hair by a vacuum
freeze-drying method with a vacuum degree of 9.5 Pa, a temperature of -50°C, and a drying
time of 48 h; and
(2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid nitrogen
freezing disintegrator on the steam-exploded and dried goat hair to obtain goat hair powder
with a particle size of 20 Iim.
[0014b] The present invention discloses goat hair powder obtained through the method above.
[0015] The present invention discloses a goat hair adsorbent, containing the goat hair powder
obtained through the method above.
[0016] The present invention discloses application of the goat hair adsorbent above in dyeing
wastewater.
[0017] The present invention discloses a method for treating dyeing wastewater with a goat
hair adsorbent, wherein the goat hair powder obtained through the method above is placed
into reactive dye dyeing wastewater for adsorption.
[0018] In an embodiment of the present invention, adsorption conditions are: pH=2 to 5, and a
time of 6 to 10 h.
[0019] In an embodiment of the present invention, a material-to-liquid ratio of the goat hair
powder to the reactive dye dyeing wastewater is 1: (50 to 100).
[0020] Beneficial effects of the present invention are as follows.
[0021] (1) The combined treatment of steam explosion and disintegration used in the present
invention is an efficient and environment-friendly pretreatment method, and compared with
waste goat hair, the treated goat hair has the powder particles of as low as 15 im and the
4a crystal index of as low as 2.6%, which increases the amorphous region of the goat hair powder,
the BET specific surface area of steam exploded and liquid nitrogen disintegrated goat hair is
increased from 0.6777 to 8.5829 m 2 g-1, the BJH adsorption cumulative surface area of pores is
increased from 0.269 m2 g-1 to 5.539 m 2g-1, the volume of pores is increased from 0.170 to 5.41
mm3 g-1, which is superior to the sum of the improvement effects of steam explosion alone and
disintegration alone on the BET specific surface area, the BJH adsorption cumulative surface
area of pores, and BJH adsorption cumulative volume of pores, indicating that the steam
explosion and the disintegration support each other and complement each other in increasing
the specific surface area and pore volume of the goat hair, and are beneficial to the adsorption
of the goat hair.
[0022] (2) The goat hair adsorbent prepared by the method of the present invention adsorbs
dye RB19 in the dyeing wastewater, and the adsorption capacity can reach 426 mg/g, which is
an excellent biological adsorbent.
[0023] (3) The goat hair adsorbent prepared by the method of the present invention can repeat
adsorption-desorption cycles 5-6 times.
Brief Description of Figures
[0024] Fig.1 is SEM images (x800) of different treatments of goat hair; the pressure and time
shown in the figure are the conditions of steam explosion, which are all samples after the
combined treatment of steam explosion and disintegration; CGH is the image of waste goat hair;
FDGH is alone disintegration treatment; EGHP is the combined treatment of steam explosion
and disintegration.
[0025] Fig.2 is XRD spectra of goat hair after the different steam explosion conditions.
[0026] Fig.3 is BET adsorption-desorption isotherm. Including, a: waste goat hair, b: liquid
nitrogen disintegrated goat hair, c: goat hair treated by steam explosion and disintegration
under 1.3MPa, d: goat hair treated by steam explosion and disintegration under 1.5MPa, e:
goat hair treated by steam explosion and disintegration under 1.7MPa.
[0027] Fig.4 is the effect of explosion conditions on adsorption capacity.
[0028] Fig.5 is the relationship between the number of cycles of adsorption and the amount of
adsorption.
[0029] Fig.6 is the adsorption performance of different treatments of goat hair: (a) ~(c) are the
effects of initial dye concentration on the Removal efficiency and adsorption at equilibrium of
different treatments of goat hair. (a) waste goat hair; (b) liquid nitrogen disintegrated goat hair;
(c) goat hair treated by steam explosion and disintegration; (d) ~ (f) are Langmuir and
Freundlich adsorption isotherm curves toward RB19. Including, (d) waste goat hair, (e) liquid
nitrogen disintegrated goat hair and (f) goat hair treated by steam explosion and disintegration.
Detailed Description
[0030] The crystal index (CI) of the samples was calculated based on the Segal's equation.
I o-Io
[0031] CI(%) 914 x 100 (1)
[0032] Where I9 is the intensity of absorption peak at 20 =9 and I 4is the intensity of
absorption valley at 20 =14.
Example 1
[0033] Using steam explosion and disintegration with the liquid nitrogen freezing disintegrator
to treat waste goat hair, comprising the following steps:
[0034] Step 1: Using steam explosion to pretreat waste goat hair:
[0035] (1) performing steam explosion on the waste goat hair, wherein the steam explosion
pressure is 1.5 MPa, and the steam explosion time is 150 s; and
[0036] (2) filtering to remove water in the steam-exploded goat hair with a 200 mesh screen;
and
[0037] (3) placing the steam-exploded sample in an ultra-low temperature refrigerator at -80°C
for 2 h, and then drying the goat hair by a vacuum freeze-drying method with a vacuum degree
of 9.5 Pa, a temperature of -50°C, and a drying time of 48 h; and
[0038] Step 2: disintegration with the liquid nitrogen freezing disintegrator: performing the
liquid nitrogen freezing disintegrator on the steam-exploded and dried goat hair to obtain goat
hair powder with a particle size of 20 im. The goat hair has a small size and small voids inside,
which has a strong adsorption effect.
[0039] Step 3: Using the goat hair powder prepared above to treat dyeing wastewater:
[0040] (1) placing the goat hair powder by steam-exploded and disintegrated into reactive dye
19 dyeing wastewater for adsorption, which adsorption conditions are pH=2, 8 hours at 21°C,
and the amount of the steam-exploded goat hair is 10g/L;
[0041] (2) Using the No. 5 sand core funnel to filter to obtain purified water and goat hair
adsorbing reactive blue 19 dye.
Example 2: Effect of different steam explosion conditions on the properties of goat wool
powder
[0042] 1. The influence of different steam pressure on goat hair performance:
[0043] The method of Example 1 was used to treat waste goat hair. The only difference was
that the steam flash explosion pressure was 1.3 MPa and 1.7 MPa, and the particle size of the
goat hair obtained after treatment was about 36im and 18 pm, respectively. The adsorption
performance and the crystal index of goat hair are shown in Fig. 4, Table 1 and Table 2.
[0044] 2. The influence of different steam treatment time on goat hair performance:
[0045] The method of Example 1 was used to treat waste goat hair. The only difference was
that the steam treatment time was 30 s, 90 s, and 240 s, and the particle sizes of the goat hair
obtained after treatment were 42 m, 38 pm, and 19 m. The adsorption performance and
crystal index of goat hair are shown in Fig. 4 and Table 2.
[0046] Table 1 Effect of different steam explosion conditions on the properties of goat wool
powder
Steam pressure Steam treatment Crystal Relative Crystal Group Ii Iii /MPa time/s Index Index Control 0 150 3342 2337 30.1 100 Al 1.3 150 2189 2012 8.1 27 A2 (Example 1.5 150 2062 1951 5.4 18 1)
A3 1.7 150 2011 1959 2.6 8.6 Control 1.5 0 3342 2337 30.1 100 BI 1.5 30s 2138 1977 8 26.5 B2 1.5 90s 2063 1935 6.2 20.6 B3 1.5 240s 2067 1959 5.2 17.3
[0047] It can be seen from Fig. 1 that the scales of goat hair are destroyed under the steam
condition of 1.3 MPa, 1.5 MPa and 1.7 MPa. As the steam pressure increases, the scales of goat hair are damaged more seriously. Therefore, it is expected that in the process of adsorption of
RB19 by steam exploded goat hair, the dye will more easily enter the amorphous region of goat
hair without the hindrance of scales to improve the adsorption performance. At the same time,
more adsorption sites of goat hair are exposed after the scales are destroyed. This is also an
important factor of improving the adsorption performance of steam exploded goat hair. The
microscopic surface scales of goat wool are destroyed when treated with 30s, 90s, 150s and
240s, however, the damage of scales slightly increased with the extended steam treatment
time. After the goat hair treated with liquid nitrogen, the size becomes smaller, and the specific
surface area of goat hair increases, leading to exposing more adsorption sites and further
improvement of the adsorption performance. At the same time, adsorbent with small particles
usually have a higher specific surface area than that with large particles, which can expose
more available adsorption active sites, thus leading to higher adsorption. In this study, the goat
hair with smaller size (<150pim) has stronger adsorption performance for RB19 than the
centimeter-sized goat hair. Particle size is only one aspect, scale destruction, crystallinity, and
pore size are also reasons for the increase in adsorption capacity.
[0048] As can be seen from Fig. 4, the adsorption capacity of goat hair obviously increased with
the increased steam pressure from 1.3 to 1.8 MPa. The adsorption capacity of goat hair under
the steam explosion of 1.3 MPa, 1.5 MPa and 1.7 MPa is 286.4 mg/g, 385.8 mg/g and 426.7
mg/g, respectively. The adsorption capacity of the goat hair treated with steam explosion and
liquid nitrogen under 1.3 MPa, 1.5 MPa, 1.7 MPa, is about 5, 7, 8 times of waste goat hair.
However, the extension of the treatment time will not bring about a significant increase in the
adsorption capacity.
[0049] It can be seen from Table 1 and 2 that the crystal index of waste goat hair is 30.1%, and
the crystal index of goat hair decreases after a certain steam pressure. The crystallization
indices of the goat hair treated with steam explosion under the pressure of 1.3 MPa, 1.5 MPa and 1.7 MPa and treatment time of 150 s are 8.1%, 5.4%, and 2.6%, respectively. Therefore, it indicated that the amorphous region of goat hair expanded after the steam explosion, so that more RB19 molecules could be adsorbed into the expanded amorphous region of exploded goat hair, and the adsorption capacity improved. Moreover, as the steam pressure changes from 1.3
MPa to 1.7 MPa, the crystal index of flash goat hair is further reduced, and the internal
amorphous region of exploded goat hair is further expanded. This promotes the further
improvement of the adsorption capacity of exploded goat hair to RB19. However, under a
certain steam pressure, the crystal index of steam explosion goat hair does not decrease
significantly with the extension of the treatment time. Therefore, it can be said that treatment
time has no obvious promoting effect on the ability of exploded goat hair to absorb dyes.
Generally speaking, as for goat hair, steam pressure is the key factor to improve the adsorption
capacity of goat hair to RB19.
[0050] Example 3: Reuse of goat hair adsorbent
[0051] Desorption and repeated adsorption of goat hair adsorbent include the following steps:
[0052] (1) Wash the goat hair after adsorbing the dye inO.1g/L NaOH for 30 minutes to achieve
desorption;
[0053] (2) subsequently washed with distilled water till neutral, and freeze-dry the collected
desorbed goat hair again;
[0054] (3) Repeatedly adsorb the desorbed goat hair. The adsorption conditions are the same
as those in step 3 in Example 1. The result is shown in Fig. 5 that goat wool adsorbent can
repeat the adsorption and desorption cycle 5-6 times.
[0055] Comparative example 1:
[0056] The original abandoned goat hair without any treatment, the SEM image, XRD image,
adsorption performance and crystal index of goat hair are shown in Figure 1, 2, 6 and Table 1-3.
[0057] Comparative example 2: separate treatment of steam explosion
[0058] The method of Example 1 was used to treat waste goat hair. The difference is that the
waste goat hair was treated separately by steam explosion under 1.5MPa and 150s. The size of
the goat hair obtained was 20 pm. The SEM image, XRD image, performance of adsorption and
crystal index are shown in Figure 1, 2, 6 and Table 1-3.
[0059] Comparative example 3: separate treatment of the liquid nitrogen freezing
disintegrator
[0060] The method of Example 1 was used to treat waste goat hair. The difference is that the
waste goat hair was treated separately by the liquid nitrogen freezing disintegrator. The
particle size of the obtained goat hair was 150 m. The SEM image and specific surface area
adsorption performance of goat hair are shown in Fig. 1 and Table. 3 and Fig. 4.
[0061] Table. 2 surface area and pore size of goat wool after different treatment
BET specific BJH adsorption BJH adsorption BJH adsorption Sample surface Area cumulative surface cumulative volume of average pore width m 2 /g area of pores m 2/g pores cm 3/g (4V/A)
Comparative 0.6777 0.269 0.000170 25.332A example 1
Comparative 1.0544 0.310 0.00175 22.601A example 2
Comparative 0.7777 0.369 0.000270 26.132A example 3
Al 3.0520 2.187 0.002091 38.244A
Example 1 4.4102 3.189 0.003405 42.720A
A3 8.5829 5.539 0.005419 39.134A
[0062] Table. 3 adsorption ability of goat wool after different treatment
BJH adsorption Adsorption Sample Diameter /pm Crystal index cumulative volume of poresm 3 /g capacity (mg/g) pores cm 3/
Comparative 1001pm 30.1 0.000170 55 example 1
Comparative 60 8.5 0.00175 180 example 2
Comparative 150 29.5 0.000175 124 example 3
Al 36 8.1 0.002091 286
Example 1 20 5.4 0.003405 426
A3 18 2.6 0.005419 326
[0063] It can be seen from Table 2 that compared with Comparative Example 1 (blank group),
the BET specific surface area and BJH adsorption cumulative surface area of pores of the steam
exploded goat hair powder in Comparative Example 2 increased by 0.3767 m 2 /g and 0.041
m 2/g, respectively. Comparing with Comparative Example 1 (blank group), the BET specific
surface area and BJH adsorption cumulative surface area of pores of the liquid nitrogen
disintegrated goat hair powder in Comparative Example 3 increased by 0.1 m 2 /g and 0.1m 2/g,
respectively. While, Comparing with Comparative Example 1 (blank group), the BET specific
surface area and BJH adsorption cumulative surface area of pores of steam exploded and liquid
nitrogen disintegrated goat hair powder in Example 1 were increased by 3.7325 m 2 /g and 1.918
m 2/g, respectively. It is superior to the sum of the improvement effects of steam explosion
alone and disintegration alone on the BET specific surface area and the BJH adsorption
cumulative surface area of pores (0.4767 m 2 /g and 0.141 m 2/g), indicating that the steam
explosion and the disintegration support each other and complement each other in increasing the specific surface area and pore volume of the goat hair, and are beneficial to the adsorption of the goat hair.
[0064] It can be seen from Table 3 that compared with Comparative Example 1 (blank group),
the goat hair obtained by steam explosion treatment alone (comparative example 2) has an
adsorption capacity of 180 mg/g for dyes, which is 125 mg/g higher than that of comparative
example 1 (blank group). The goat hair obtained by disintegration alone (Comparative Example
3) has an adsorption capacity of 124mg/g for dyes, which is 69 mg/g higher than that of
Comparative Example 1 (blank group). Example 1 was obtained by the combined treatment of
steam flash explosion and disintegration has an adsorption capacity of 426 mg/g for dyes,
which has an increase of 371 mg/g compared with Comparative Example 1 (blank group). It is
superior to the sum of the improvement effects of steam explosion alone and disintegration
alone on the dye adsorption capacity (194 mg /g), indicating that the steam explosion and the
disintegration support each other and complement each other in increasing the specific surface
area and pore volume of the goat hair, and are beneficial to the adsorption of the goat hair. The
crystallization index of goat hair treated by steam explosion alone is 8.5, and the crystallization
index of goat hair by disintegration alone is 29.5, while the steam exploded and liquid nitrogen
disintegrated goat hair is 5.4. It indicates that disintegration alone does not change the
crystallinity of goat hair.
[0065] The reference to any prior art in this specification is not, and should not be taken as, an
acknowledgement or any form of suggestion that such prior art forms part of the common
general knowledge.
[0066] It will be understood that the terms "comprise" and "include" and any of their
derivatives (e.g. comprises, comprising, includes, including) as used in this specification, and the
claims that follow, is to be taken to be inclusive of features to which the term refers, and is not
meant to exclude the presence of any additional features unless otherwise stated or implied.
[0067] In some cases, a single embodiment may, for succinctness and/or to assist in
understanding the scope of the disclosure, combine multiple features. It is to be understood
that in such a case, these multiple features may be provided separately (in separate
embodiments), or in any other suitable combination. Alternatively, where separate features are
described in separate embodiments, these separate features may be combined into a single
embodiment unless otherwise stated or implied. This also applies to the claims which can be
recombined in any combination. That is a claim may be amended to include a feature defined in
any other claim. Further a phrase referring to "at least one of" a list of items refers to any
combination of those items, including single members. As an example, "at least one of: a, b, or
c" is intended to cover: a, b, c, a-b, a-c, b-c, and a-b-c.
[0068] It will be appreciated by those skilled in the art that the disclosure is not restricted in its
use to the particular application or applications described. Neither is the present disclosure
restricted in its preferred embodiment with regard to the particular elements and/or features
described or depicted herein. It will be appreciated that the disclosure is not limited to the
embodiment or embodiments disclosed, but is capable of numerous rearrangements,
modifications and substitutions without departing from the scope as set forth and defined by
the following claims.
Claims (13)
1. A method for preparing an efficient dyeing wastewater adsorbent from waste goat hair,
comprising: treating the waste goat hair using a combination of steam explosion and
disintegration with the liquid nitrogen freezing disintegrator to obtain goat hair powder as the
adsorbent for treating dyeing wastewater.
2. The method according to claim 1, wherein steam explosion conditions are: an explosion
pressure of 1.3 MPa to 1.7 MPa, and an explosion time of 30 s to 240 s.
3. The method according to either claim 1 or claim 2, wherein the method comprises the
following steps:
(1) steam explosion: performing steam explosion on the waste goat hair, and freeze-drying; and
(2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid nitrogen
freezing disintegrator on the goat hair in step (1) to obtain the goat hair powder.
4. The method according to claim 3, wherein the method comprises the following steps:
(1) steam explosion: performing steam explosion on the waste goat hair, sieving with a 200 to
300 mesh sieve, and then freeze-drying; and
(2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid nitrogen
freezing disintegrator on the goat hair in step (1) to obtain goat hair powder with a particle size
of 10 to 30 pm.
5. The method according to either claim 3 or claim 4, wherein the freeze-drying in step (1) is to
freeze the steam-exploded sample at -60 to -80°C for 1to 4 h, and then dry the goat hair by
vacuum freeze-drying.
6. The method according to claim 5, wherein vacuum freeze-drying conditions are: a vacuum
degree of 5 to 15 Pa, a temperature of -40 to -60°C, and a drying time of 36 to 72 h.
7. The method according to any one of claims 1 to 6, wherein the method comprises the
following steps:
(1) steam explosion: performing steam explosion on the waste goat hair, wherein a steam
explosion pressure is 1.5 MPa, and a steam explosion time is 150 s; filtering to remove water in
the steam-exploded goat hair with a 200 mesh screen; placing the steam-exploded sample in an
ultra-low temperature refrigerator at -80°C for 2 h, and then drying the goat hair by a vacuum
freeze-drying method with a vacuum degree of 9.5 Pa, a temperature of -50°C, and a drying
time of 48 h; and
(2) disintegration with the liquid nitrogen freezing disintegrator: performing the liquid nitrogen
freezing disintegrator on the steam-exploded and dried goat hair to obtain goat hair powder
with a particle size of 20 im.
8. Goat hair powder prepared by applying the method according to any one of claims 1 to 7.
9. A goat hair adsorbent, containing the goat hair powder according to claim 8.
10. Use of the goat hair adsorbent according to claim 9 in dyeing wastewater.
11. A method for treating dyeing wastewater with a goat hair adsorbent, comprising: placing
the goat hair powder according to claim 8 into reactive dye dyeing wastewater for adsorption.
12. The method according to claim 11, wherein adsorption conditions are: pH=2 to 5, and a
time of 6 to 10 h.
13. The method according to either claim 11 or claim 12, wherein a material-to-liquid ratio of
the goat hair powder to the reactive dye dyeing wastewater is 1: (50 to 100).
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Jia, F. et al. "Effect of steam explosion on the structures and properties of waste coarse goat fibers" Wool Textile Journal, 28 February 2019, vol. 47, no. 2, pages 25-29 * |
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