CN113149551B - Superfine sulfur-containing tailing concrete - Google Patents
Superfine sulfur-containing tailing concrete Download PDFInfo
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- CN113149551B CN113149551B CN202110403046.8A CN202110403046A CN113149551B CN 113149551 B CN113149551 B CN 113149551B CN 202110403046 A CN202110403046 A CN 202110403046A CN 113149551 B CN113149551 B CN 113149551B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses superfine sulfur-containing tailing concrete, which comprises the following raw materials: low clinker cement and superfine sulfur-containing tailings. The invention uses M32.5 low clinker composite cement as cementing material, and uses the equal volume of the superfine sulfur-containing tailings to replace cement and water, thereby realizing the preparation of the superfine sulfur-containing tailings high-doped concrete. The invention fully utilizes the sulfate released by the acidification of the sulfide of the superfine sulfur-containing tailings to excite the high-quantity auxiliary materials of the M32.5 cement, improves the bonding strength, improves the economic value of the superfine sulfur-containing tailings to the level of the M32.5 cement, changes waste into valuable and changes the harm into the treasure. The concrete of the invention has stable mechanical property and micro-expansion. The method is simple to operate, low in cost and wide in application prospect under the background of shortage of building material market raw materials.
Description
Technical Field
The invention relates to the field of resource utilization of sulfur-containing tailings, and in particular relates to superfine sulfur-containing tailing concrete.
Background
Tailings are industrial solid wastes discharged in the process of sorting operation after ore mining, and are huge in quantity. Statistically, the discharge amount of iron tailings only reaches about 120 hundred million m in the whole country 3 . Such a huge amount of tailings not only occupy the land by piling up, but also seriously pollute the soil, water resources, air and the like, but also need to invest a large amount of capital for the maintenance and operation of a tailing pond. Therefore, the resource utilization of the tailings becomes a consensus of all communities, and is also a key direction of the recycling of industrial solid waste resources in China at present.
However, tailings discharged from the non-ferrous metal industry often accompany a large amount of sulfides (mainly pyrites, feS) 2 ) Higher sulfur content (converted to SO) 3 More than 1% by mass), fine particles and high difficulty in large-scale utilization. Currently, how to effectively utilize the superfine sulfur-containing tailings has become an interest for enterprises and governmentsThe focus of (2).
Generally, the tailing is made into concrete, which is an effective way for realizing large-scale tailing digestion. However, for sulfur-containing tailings, when high clinker cements (e.g., p.o.42.5, p.o.52.5, etc.) are used, the clinker content>70%) of the sulfur-containing tailings, the volume of the concrete is often unstable, the performance of the hydration product is deteriorated, the compressive strength is remarkably reduced, and the like, due to incompatibility of the sulfur-containing tailings and the sulfur-containing tailings. As shown in formula (1), pyrite in the sulfur-containing tailings is oxidized after meeting water to form iron oxide and sulfate, and a certain amount of H is released + . The sulphate formed after acidification of the pyrite will then attack the cement hydration product Ca (OH) 2 The reaction as shown in formula (2) occurs and gypsum is formed, so that Ca (OH) in the gelling system is formed 2 Reduced content of Ca (OH) 2 The stability of the crystal is deteriorated, the C-S-H (the main hydration product of cement) stabilizes the environmental change, and the gel performance is deteriorated. At the same time, the gypsum formed according to formula (2) also reacts with tricalcium silicate (3 CaO. Al) in the unhydrated cement particles 2 O 3 ) The reaction promotes a large amount of expansive ettringite crystals (3 CaO. Al) 2 O 3 ·3CaSO 4 ·32H 2 O) causes the concrete to obviously expand and even burst and break, and seriously affects the safety and durability of concrete materials and structures.
3CaO·Al 2 O 3 +3CaSO 4 ·2H 2 O+30H 2 O→3CaO·Al 2 O 3 ·3CaSO 4 ·32H 2 O (forming ettringite) (3)
Therefore, the biggest difficulty in preparing concrete by using sulfur-containing tailings is how to avoid incompatibility between cement clinker and sulfur-containing tailings oxysulfate, and a great deal of research work is carried out by domestic and foreign scholars. In view of the yellow iron in the sulfur-containing tailingsThe oxidation of ore is an inevitable natural phenomenon, the sulfur-containing tailings can be cemented by alkali-activated cementing materials, and sulfate oxide of the sulfur-containing tailings is used as an additional activator and is mixed with alkali salt (NaOH and Na) 2 SO 4 、 Na 2 CO 3 Water glass, etc.) to promote the depolymerization of the cementing material (including flyash, blast furnace slag, slag ash, etc.) and to form three-dimensional netted Si-O-Al-Si-O, al-O bond under the action of alkali and salt]The structural system or the C- (A) -S-H gel product improves the mechanical strength and durability of the cement body. The advantages of using the glue include: 1) Green: industrial solid waste is used as a cementing material, and the additional excitation function of sulfide oxidized sulfate of sulfur-containing tailings is utilized in a synergistic manner, so that the energy is saved and the environment is protected; 2) Excellent performance: the alkali-activated material is a clinker-free cementing material, has low hydration heat, excellent pore structure (the alkali slag material also has the advantages of quick hardening, early strength and the like), and good durability; 3) The special purpose is as follows: the alkali-activated material is high-temperature resistant (the performance of the alkali-activated material is still stable under the environment of 600 ℃), and the high-alkali environment and the gelled product have strong heavy metal curing capacity, so that the alkali-activated material is also suitable for high-temperature or heavy metal polluted environments. However, the performance of the alkali-activated material is not fully mature, the research and application have a large distance, and the market acceptance is low (only a few buildings or airports in the whole world adopt the alkali-activated material, and only 3 relevant standards are issued in China). However, if the alkali-activated material is directly adopted to cement the sulfur-containing tailings to prepare the concrete, the popularization and the application of the sulfur-containing tailings-based concrete product are seriously influenced, and the resource utilization of the sulfur-containing tailings is limited.
Disclosure of Invention
The invention aims to solve the problems in the prior art, low-clinker cement is used as a cementing material, superfine sulfur-containing tailings are used as a slurry substitute for cement and water, sulfate radicals released by acidification of the superfine sulfur-containing tailings are used for assisting in exciting low-clinker cement auxiliary materials to form a reinforced cementing body, waste is changed into valuable, harm is changed into valuable, and the economic value of the superfine sulfur-containing tailings is greatly improved.
The technical scheme adopted by the invention is as follows: the superfine sulfur-containing tailing concrete comprises the following raw materials: low clinker cement and superfine sulfur-containing tailings.
As a further improvement of the invention, the water-reducing agent also comprises water, sand, stones and water reducing agent.
As a further improvement of the invention, the composition in parts by weight is as follows: 189-409 parts of cement, 74-226 parts of superfine sulfur-containing tailings, 140-370 parts of water, 669-956 parts of sand, 762-1226 parts of stones and 3.9-17.3 parts of water reducing agent.
As a further improvement of the invention, the low clinker cement is an M32.5 compound cement.
As a further improvement of the invention, the fineness of the superfine sulfur-containing tailings is-200 meshes and accounts for more than 70%.
As a further improvement of the invention, the water reducing agent is a polycarboxylic acid high-efficiency water reducing agent.
As a further improvement of the invention, the superfine sulfur-containing tailings contain sulfur (converted into SO) 3 By mass) greater than 2%.
The invention has the following beneficial effects: the invention has the following advantages: 1) M32.5 is a commercial cement with a low clinker content: (<50%) and more supplementary cementitious material (including lime, fly ash, blast furnace slag, slag ash, etc.). When the M32.5 cement and the sulfur-containing tailings are used for preparing the concrete, clinker components in the cement and water are quickly hydrated to form a stressed framework of the concrete and are gradually hardened, and compared with high-clinker cement, hydration products formed by hydration of the cement are fewer. While the sulfur-containing tailings are continuously fixed in the concrete microstructure, the periphery of the tailings contains a large amount of auxiliary gelled materials, the acidification and sulfate release processes of the tailings are long, and the continuously released sulfate can be combined with pore alkali liquor (Ca (OH) in the concrete microstructure 2 ) Forming a composite alkaline activator, promoting the silicon-oxygen tetrahedron Si-O, al-O bond in the auxiliary material to break, and polymerizing again to form a three-dimensional net [ -Si-O-Al-]Structural system or C- (A) -S-H gel product, avoiding damaging the stability of cement hydration products; 2) The sulfur-containing tailings are small in particles, are natural powder for concrete, have certain gelation effect on the concrete, can fully utilize the effect of fine particles to play a role in filling pores, and improve the concrete qualityBulk density of the soil particles; 3) At present, the price of cement is always high, M32.5 cement reaches 300-400 yuan/ton, and the economic value is high. In fact, the utilization technology and the way of the sulfur-containing tailings are more, but the economic value of the sulfur-containing tailings is the key for determining the resource utilization of the sulfur-containing tailings. The invention adopts a slurry substitution method, uses superfine sulfur-containing tailings as a slurry substitution material of cement and water, compensates the reduction of the strength of the sulfur-containing tailings concrete (the activity of the sulfur-containing tailings is lower than that of the cement, and has stronger dilution effect on the cement) by reducing the water-cement ratio, and realizes the purpose of largely consuming the sulfur-containing tailings; by the method, the economic value of the sulfur-containing tailings can be directly increased to the level of M32.5 cement, so that the method has remarkable economic, social and environmental significance for resource utilization of the sulfur-containing tailings and has wide application prospect. The concrete of the invention has stable mechanical property and micro-expansion. The method is simple to operate and low in cost, and has wide application prospect under the background of shortage of raw materials in the building material market.
Detailed Description
The present invention will be further described with reference to the following examples.
The superfine sulfur-containing tailing concrete comprises the following raw materials: low clinker cement and superfine sulfur-containing tailings.
Further, the water-reducing agent comprises water, sand, stones and a water reducing agent, and the water-reducing agent comprises the following components in parts by weight: 189-409 parts of cement, 74-226 parts of superfine sulfur-containing tailings, 140-370 parts of water, 669-956 parts of sand, 762-1226 parts of stones and 3.9-17.3 parts of water reducing agent.
In 2018, 11 and 19, the general administration of market supervision and management in China and the national committee of standardization and management approved GB175-2007 Portland Universal Cement No. 3 modification order, the 32.5 strength grade (PC32.5R) of the composite Portland cement is cancelled, the four strength grades of 42.5, 42.5R, 52.5 and 52.5R are reserved after modification, and the implementation is carried out in 2019, 10 and 1. In spite of the situation of cement enterprises, large-scale domestic cement enterprises successively push out M32.5 cement, and the M32.5 cement replaces P.C32.5 cement to the market. Although the M32.5 cement and the PC32.5R grade cement have the same grade of strength, the two cement have large difference.
First, the M32.5 cement does not define a magnesium oxide and alkali content control range, and if used to produce structural concrete, there would be a safety quality risk. In addition, the setting time of the M32.5 cement is relatively long, and the construction progress of the project is influenced to a certain extent.
Secondly, the mixing amount of the M32.5 cement auxiliary material has no upper limit or lower limit, and even the auxiliary material can be completely used for production, so the early strength is lower than that of the P.C32.5R cement.
In order to improve the economic value of the superfine sulfur-containing tailings, the superfine sulfur-containing tailings are used for replacing cement and water in equal volume, namely the use amount of the cement is reduced, and meanwhile, a large amount of the superfine sulfur-containing tailings are fully utilized. Meanwhile, sulfate released by acidification of superfine sulfur-containing tailing sulfide is used for exciting high-quantity auxiliary materials of M32.5 cement, and the bonding strength is improved.
Example 1: a superfine sulfur-containing tailing concrete comprises M32.5 cement, superfine sulfur-containing tailing, sand, pebbles, a water reducing agent and water. The specific weight parts (kg) ratio is shown in Table 1,
TABLE 1
Wherein: the density of the M32.5 cement is 3.1g/cm 3 (ii) a The fineness modulus of the sand was 2.5; the superfine sulfur-containing tailings are sieved by a 200-mesh sieve, the average grain diameter is 76 microns, and the density is 3.06g/cm 3 Sulfur content (converted to SO) 3 By mass,%) 3.37%; the stones are 10-20 mm continuous size fraction limestone; the water is tap water with a density of 1g/cm 3 (ii) a The water reducing agent is a polycarboxylic acid high-performance water reducing agent; the slurry substitution rate is the volume of the superfine sulfur-containing tail substituted mortar (the volume of M32.5 cement and water).
Concrete is prepared according to the proportion shown in the table 1, poured into a cubic steel mold with the side length of 150mm, and placed into a standard curing room with the temperature of 20 +/-2 ℃ and the relative humidity of more than 95 percent for curing for 1 day. Thereafter, the test block was demolded and maintained for 3, 7, 28 and 56 days of age, respectively. The compression strength of the superfine sulfur-containing tailing concrete of different ages is tested by using a press machine, 3 test blocks form a group, and the test results are averaged. Table 2 shows the compressive strength (MPa) of the 6 baseline groups.
TABLE 2
We can see that the effect of using the superfine sulfur-containing tailings instead of different proportions of slurry volume (the sum of the volumes of cement and water) on the compressive strength of the superfine sulfur-containing tailings concrete has a certain regularity: along with the increase of the substitution rate, the compressive strength of the superfine sulfur-containing tailing concrete at each age is increased firstly and then reduced. When the substitution rate was 12% (reference group 4), the compression strengths of reference group 4 were all greater than those of reference group 1 for 3 days, 7 days, 28 days, and 56 days. In the course of the experiment, no expansion phenomenon was found in the test block, and it was also found from table 4 that the compression strength of the ultrafine tailing concrete did not suffer deterioration with age. This fully proves the technical reliability of the ultra-fine sulfur-containing tailing concrete provided by the invention.
Example 2:
the invention provides superfine sulfur-containing tailing concrete which comprises M32.5 cement, superfine sulfur-containing tailing, sand, stones, a water reducing agent and water. The specific weight parts (kg) formulation is shown in table 3,
TABLE 3
Wherein: the density of the M32.5 cement is 3.1g/cm 3 (ii) a The fineness modulus of the sand was 2.5; the superfine sulfur-containing tailings are sieved by a 200-mesh sieve, the average grain diameter is 76 microns, and the density is 3.06g/cm 3 Sulfur content (converted to SO) 3 By mass,%) 3.37%; the stones are 10-20 mm continuous size fraction limestone; the water is tap water with a density of 1g/cm 3 (ii) a The water reducing agent is polycarboxylic acid high-performanceCan reduce water agent. Wherein the slurry substitution rate is the volume of the superfine sulfur-containing tail substituted mortar (the volume of M32.5 cement and water).
Concrete was prepared according to the formulation shown in table 3, poured into a cubic steel mold with side length of 150mm, and placed in a standard curing room with a temperature of 20 ± 2 ℃ and a relative humidity of more than 95% for curing for 1 day. Thereafter, the test block was demolded and maintained for 3, 7 and 28 days of age, respectively. And (3) testing the compressive strength of the ultrafine sulfur-containing tailing concrete of different ages by using a press, wherein 3 test blocks form a group, and the test results are averaged. Table 4 shows the compressive strength (MPa) of the 3 baseline groups.
TABLE 4
According to the specification of GB50010 'concrete structure design specification' on concrete strength grades, the concrete strength grades of the reference group 7, the reference group 8 and the reference group 9 are respectively C30, C35 and C40, and the use requirements of related projects are met.
The invention has the following advantages: 1) M32.5 is a commercial cement with a low clinker content: (<50%), more auxiliary cementing materials (including lime, fly ash, blast furnace slag, cinder ash, etc.). When the M32.5 cement and the sulfur-containing tailings are used for preparing concrete, clinker components in the cement are quickly hydrated with water to form a stressed framework of the concrete and are gradually hardened, and compared with high-clinker cement, the hydration products formed by hydration of the cement are fewer. While the sulfur-containing tailings are continuously fixed in the concrete microstructure, the periphery of the tailings contains a large amount of auxiliary gelling materials, the acidification and sulfate release processes of the tailings are long, and the continuously released sulfate can be combined with pore alkali liquor (Ca (OH) in the concrete microstructure 2 ) Forming a composite alkaline activator to promote the breakage of silicon-oxygen tetrahedron Si-O, al-O bonds in the auxiliary materials and repolymerization to form a three-dimensional net [ -Si-O-Al-]Structural systems or C- (A) -S-H gel products, so as to avoid damaging the stability of cement hydration products; 2) The sulfur-containing tailings are small in particle, are natural powder for concrete and are used for concreteNot only has certain gelation, but also can fully utilize the fine particle function to play a role in filling pores, thereby improving the bulk density of concrete particles; 3) At present, the price of cement is always high, M32.5 cement reaches 300-400 yuan/ton, and the economic value is higher. In practice, there are many techniques and ways to utilize sulfur-containing tailings, but the economic value of sulfur-containing tailings is the key to determine the resource utilization. The invention adopts a slurry substitution method, uses superfine sulfur-containing tailings as a slurry substitution material of cement and water, compensates the reduction of the strength of the sulfur-containing tailings concrete (the activity of the sulfur-containing tailings is lower than that of the cement, and has stronger dilution effect on the cement) by reducing the water-cement ratio, and realizes the aim of greatly consuming the sulfur-containing tailings; by the method, the economic value of the sulfur-containing tailings can be directly increased to the level of M32.5 cement, so that the method has obvious economic, social and environmental significance for resource utilization of the sulfur-containing tailings and has wide application prospect. The concrete of the invention has stable mechanical property and micro-expansion. The method is simple to operate, low in cost and wide in application prospect under the background of shortage of building material market raw materials.
It is understood by those skilled in the art that the protection scheme of the present invention is not limited to the embodiments described above, and various permutations and modifications can be made on the above embodiments without departing from the spirit of the invention.
Claims (2)
1. The superfine sulfur-containing tailing concrete is characterized by comprising the following components in parts by weight: 189-409 parts of low clinker cement, 74-226 parts of superfine sulfur-containing tailings with the average particle size of 76 microns, 140-370 parts of water, 669-956 parts of sand with the fineness modulus of 2.5, 762-1226 parts of stones and 3.9-17.3 parts of a water reducing agent; wherein: the low clinker cement is M32.5 composite cement, the M32.5 composite cement comprises cement clinker and auxiliary material components, the auxiliary material is a substance containing Si-O bonds and Al-O bonds, and the content of the cement clinker in the M32.5 composite cement is less than 50%; the superfine sulfur-containing tailings contain sulfide FeS 2 The sulfur content of the superfine sulfur-containing tailings is convertedTo SO 3 Greater than 2% by mass.
2. The ultrafine sulfur-containing tailing concrete according to claim 1, wherein the water reducer is a polycarboxylic acid high-efficiency water reducer.
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| CN114560660A (en) * | 2022-03-15 | 2022-05-31 | 安徽理工大学 | Pervious concrete prepared from copper tailings |
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| CN1872517A (en) * | 2006-04-19 | 2006-12-06 | 中国科学院广州地球化学研究所 | Method for preparing laying material from ore tailing rich in sulfur |
| CN112479617A (en) * | 2020-12-18 | 2021-03-12 | 安徽科博建材科技有限公司 | Additive for high-sulfur tailing filling cementing material and production process thereof |
| CN112551985A (en) * | 2020-12-17 | 2021-03-26 | 安徽理工大学 | Application of superfine tailings in concrete |
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| CN1099389C (en) * | 2000-03-31 | 2003-01-22 | 成县加气混凝土制品厂 | Aerocrete made of industrially desulfurized Pb-Zn tailings and its production technology |
| CN1295178C (en) * | 2004-06-25 | 2007-01-17 | 中南大学 | Method and system for treating high sulfur contained tails as binding filler aggregates |
| KR20130034716A (en) * | 2011-09-29 | 2013-04-08 | 한미이엔씨 주식회사 | Materials supplying device and the method for concrete having sulfur |
| CN105565735B (en) * | 2015-11-30 | 2018-05-18 | 北京建研昆仑科技有限公司 | Sulfur-bearing tailings curing agent and sulfur-bearing tailing cemented filling material and the consolidated fill method of mine worked-out section |
| CN110002808A (en) * | 2019-05-17 | 2019-07-12 | 辽宁工程技术大学 | A kind of alkali-activated material solidification iron tailings sand and preparation method thereof and application method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1872517A (en) * | 2006-04-19 | 2006-12-06 | 中国科学院广州地球化学研究所 | Method for preparing laying material from ore tailing rich in sulfur |
| CN112551985A (en) * | 2020-12-17 | 2021-03-26 | 安徽理工大学 | Application of superfine tailings in concrete |
| CN112479617A (en) * | 2020-12-18 | 2021-03-12 | 安徽科博建材科技有限公司 | Additive for high-sulfur tailing filling cementing material and production process thereof |
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Effective date of registration: 20230406 Address after: 244000 No.8, Aiguo Road, Tongguan District, Tongling City, Anhui Province Patentee after: Anhui Tongguan Industrial Technology Research Institute Co.,Ltd. Address before: 244000 Changjiang West Road, Anhui, Tongling Patentee before: TONGLING NONFERROUS METALS GROUP Co.,Ltd. |