原生型无水石膏在硅酸盐水泥中的作用研究
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摘要
近年来，熟料和混合材中原生硫酸盐的含量呈现上升的趋势，但为了避免硫酸盐可能带来的负面影响，世界各国均对水泥熟料及用于水泥的混合材中SO3含量进行了限定，这使广泛存在的高硫酸盐水泥熟料和高硫酸盐火山灰质废渣将难以用于生产水泥。在这种形势下，如果可以用熟料和混合材中的硫酸盐来代替外掺石膏生产水泥，就无需对熟料和混合材中的SO3含量进行限制，只需对水泥中SO3总量进行限制即可。硅酸盐水泥熟料中的硫酸盐主要为碱金属硫酸盐、复盐、硫铝酸盐和无水石膏，混合材中的硫酸盐主要为无水石膏，在这些众多类型的原生硫酸盐中与外掺石膏性能最接近的是熟料和混合材中的无水石膏（原生型无水石膏）。因此，明确原生型无水石膏在水泥水化过程中能否发挥二水石膏的作用，是合理利用原生型无水石膏及其他类型原生硫酸盐的先决条件。
本文首先分析了水泥熟料和混合材中原生型无水石膏的存在形态及含量，发现原生型无水石膏主要来源于燃煤灰渣中的无水石膏，原生型无水石膏的溶解速度低于二水石膏，但最终溶解度高于二水石膏。通过对比各条件下制备的煅烧石膏的溶解性能，在模拟制备原生型无水石膏时，选择天然二水石膏作为石膏源，煅烧参数分别为850℃下煅烧2h和1200℃下煅烧0.5h。
将原生型无水石膏与常用的硅酸盐水泥熟料复合，系统研究了原生型无水石膏对硅酸盐水泥物理力学性能的影响，结果显示原生型无水石膏对硅酸盐水泥的标准稠度需水量影响不大，但对凝结时间有显著影响，对水泥的缓凝作用高于天然硬石膏，略低于二水石膏；原生型无水石膏对水泥具有显著的增强作用，对水泥早期强度的提高作用介于天然硬石膏和二水石膏之间；原生型无水石膏可以减少水泥在干燥条件下的收缩，对水泥的补偿收缩作用与二水石膏相近。通过分析原生型无水石膏对水泥水化速度、水化反应程度以及水化产物的影响以探索原生型无水石膏对水泥水化影响的作用机理，结果显示，原生型无水石膏在水泥液相中溶解产生硫酸根离子，同时生成一定量的钙矾石，抑制了C_3A的快速水化，从而起到延缓水泥水化的作用，而适量钙矾石的形成提高了水泥的早期强度并减少了水泥的干燥收缩；同二水石膏相比，原生型无水石膏的溶解速度较慢，造成水化早期水泥液相中硫酸根离子浓度较低、钙矾石的生成量相对较少，且钙矾石生成相对较晚，因而其抑制C_3A水化的能力弱于二水石膏。
通过掺加C_3A单矿物和固体NaOH的方式获得不同C_3A含量和碱含量的水泥，在此基础上，研究了原生型无水石膏在水泥中的作用与水泥组成的关系。结果显示，水泥中C_3A和碱含量较高时，原生型无水石膏对水泥的缓凝作用降低，且对于高C_3A含量（约12%）或高碱含量（约为1.7%）的水泥，补加一定量的原生型无水石膏并不能有效延长水泥的凝结时间；同二水石膏相比，原生型无水石膏在高C_3A和高碱水泥中并不能有效发挥提高早期强度的作用；高C_3A和高碱含量下，原生型无水石膏的溶解速度小于C_3A和碱对硫酸根离子的消耗速度，使水泥液相中硫酸根离子浓度偏低，导致钙矾石难以形成，以至于造成水泥凝结时间缩短、早期强度降低。
研究了不同养护温度（20℃、65℃及90℃）和不同养护湿度（干燥养护、密封养护及浸水养护）下原生型无水石膏在水泥中作用效果的变化规律，发现养护温度会影响原生型无水石膏在水泥中的最佳掺量，经历了早期高温养护的原生型无水石膏水泥在水化后期仍有较好的体积稳定性，但其生成延迟性钙钒石的风险要高于二水石膏水泥；养护湿度对原生型无水石膏水泥宏观性能的影响与二水石膏水泥类似，但原生型无水石膏在低成型水灰比且干燥养护条件下反应更慢，水化28d时依然有少量无水石膏存在，增加了产生延迟性钙矾石的风险。
In recent years, the content of protogenetic sulfate in cement clinker and admixturebecomes higher and higher. However, in order to avoid negative effects resulted bysulfate, the SO3content in cement clinker and admixture is limited by almost allcountries, which makes the cement clinker with high sulfate and pozzolanic sludge withhigh sulfate difficult for the production of cement. In situations such as this, if thesulfate in cement clinker and admixture can substitute for the gypsum added as cementretarder, and there is no need to limit the SO3content in cement clinker and admixture,it just needs to limit the total SO3content of cement. Sulfate minerals in cement clinkerare mainly alkaline metal sulfate, double salt, sulphoaluminate and anhydrite. Sulfateminerals in admixtures are mainly anhydrite. In so many types of protogenetic sulfate,the anhydrite existed in cement clinker and admixture has the most similar performancewith dihydrate gypsum. Therefore, whether protogenetic anhydrite can play the role ofdihydrate gypsum in cement is a precondition for the reasonable use of protogeneticanhydrite and other types of protogenetic sulfate in cement production.
Firstly, the types and content of protogenetic anhydrite in cement clinker andadmixtures were analyzed. The results show that protogenetic anhydrite is mainlyexisted in coal combustion waste. The dissolution rate of protogenetic anhydrite islower than that of dihydrate gypsum, but the dissolubility of the former is higher thanthat of the latter. By comparing dissolution property of calcined gypsum produced indifferent technology, it found that calcined gypsums by using natural dihydrate gypsumcalcined at850℃temperature for2hours and at1200℃for0.5hours can be used tosimulate protogenetic anhydrite.
Influence of protogenetic anhydrite on physical-mechanical properties of Portlandcement by mixing cement clinker with various contents of protogenetic anhydrite wasresearched. The results show that protogenetic anhydrite does not much affect waterrequirement of standard consistency of Portland cement, but significantly affect thesetting time of Portland cement. The effect of protogenetic anhydrite on settingretarding of cement is stronger than natural anhydrite, but slightly weaker thandihydrate gypsum. Protogenetic anhydrite can remarkably improve the early strength ofcement, and improvement effect is a median between natural anhydrite dihydrategypsum. Protogenetic anhydrite can reduce drying-shrinkage of cement, and the effect of protogenetic anhydrite on compensating shrinkage of cement is almost the same asthat of dihydrate gypsum, but is better than that of natural anhydrite. The research abouthydration process shows that protogenetic anhydrite releases sulphate ion which canform ettringite in the cement solution, and ettringite inhibits the quick hydration of C_3A,so that retards cement hydration. The formation of ettringite improves the early strengthof the cement and reduces dry-shrinkage of cement. Compared with dihydrate gypsum,the dissolution rate of protogenetic anhydrite is too slow to result in the lower sulphateion concentration in the early time of hydration. In addition, the formation of ettringiteis less and later. So the effect of protogenetic anhydrite on inhibition hydration of C_3Ais weaker than dihydrate gypsum.
The cements with different C_3A and alkali content were obtained by adding C_3Aand solid natrium hydroxide in cement. On that basis, the influence of cementcomposition on the role of protogenetic anhydrite in Portland cement was studied. Theresults show that the effect of protogenetic anhydrite on cement hydration andhardening is closely related to cement composition. When the C_3A and alkali content incement is higher, the setting retarding effect of protogenetic anhydrite is reduced. Andfor high C_3A (about12%) or high alkali (about1.7%) cement, it can't effectivelyprolong the setting time of cement by adding a certain amount of protogenetic anhydrite.Compared with dihydrate gypsum, protogenetic anhydrite in cement with high C_3A andhigh alkali can't effectively improve the early strength of cement. In cement includinghigh C_3A and high alkali content, the dissolution rate of protogenetic anhydrite is lowerthan the consumption rate of sulphate ion, so that sulphate ion concentration is lowerand the formation of AFt becomes difficulty, that cause the setting time of cementshortened, and the early strength reduced.
The changing rule of the role of protogenetic anhydrite in Portland cement underdifferent curing temperature (including20℃,65℃and90℃) and curing humidity(including dry-curing, seal-curing and water-curing). The results show that curingtemperature will affect the optimum dosage of protogenetic anhydrite in cement.Cement produced by protogenetic anhydrite under high temperature curing in early-agestill has better volume stability in the long age, but the risk of formation of delayedettringite is higher than that of cement produced by dihydrate gypsum. The influence ofcuring humidity on physical-mechanical properties of protogenetic anhydrite issimilarly to that of dihydrate gypsum cement. But the dissolution and hydration ofprotogenetic anhydrite under dry-curing condition become much slower, so that there is still some unreacted anhydrite in cement paste at28-days age, which increases the riskof formation of delayed ettringite.
本文首先分析了水泥熟料和混合材中原生型无水石膏的存在形态及含量，发现原生型无水石膏主要来源于燃煤灰渣中的无水石膏，原生型无水石膏的溶解速度低于二水石膏，但最终溶解度高于二水石膏。通过对比各条件下制备的煅烧石膏的溶解性能，在模拟制备原生型无水石膏时，选择天然二水石膏作为石膏源，煅烧参数分别为850℃下煅烧2h和1200℃下煅烧0.5h。
将原生型无水石膏与常用的硅酸盐水泥熟料复合，系统研究了原生型无水石膏对硅酸盐水泥物理力学性能的影响，结果显示原生型无水石膏对硅酸盐水泥的标准稠度需水量影响不大，但对凝结时间有显著影响，对水泥的缓凝作用高于天然硬石膏，略低于二水石膏；原生型无水石膏对水泥具有显著的增强作用，对水泥早期强度的提高作用介于天然硬石膏和二水石膏之间；原生型无水石膏可以减少水泥在干燥条件下的收缩，对水泥的补偿收缩作用与二水石膏相近。通过分析原生型无水石膏对水泥水化速度、水化反应程度以及水化产物的影响以探索原生型无水石膏对水泥水化影响的作用机理，结果显示，原生型无水石膏在水泥液相中溶解产生硫酸根离子，同时生成一定量的钙矾石，抑制了C_3A的快速水化，从而起到延缓水泥水化的作用，而适量钙矾石的形成提高了水泥的早期强度并减少了水泥的干燥收缩；同二水石膏相比，原生型无水石膏的溶解速度较慢，造成水化早期水泥液相中硫酸根离子浓度较低、钙矾石的生成量相对较少，且钙矾石生成相对较晚，因而其抑制C_3A水化的能力弱于二水石膏。
通过掺加C_3A单矿物和固体NaOH的方式获得不同C_3A含量和碱含量的水泥，在此基础上，研究了原生型无水石膏在水泥中的作用与水泥组成的关系。结果显示，水泥中C_3A和碱含量较高时，原生型无水石膏对水泥的缓凝作用降低，且对于高C_3A含量（约12%）或高碱含量（约为1.7%）的水泥，补加一定量的原生型无水石膏并不能有效延长水泥的凝结时间；同二水石膏相比，原生型无水石膏在高C_3A和高碱水泥中并不能有效发挥提高早期强度的作用；高C_3A和高碱含量下，原生型无水石膏的溶解速度小于C_3A和碱对硫酸根离子的消耗速度，使水泥液相中硫酸根离子浓度偏低，导致钙矾石难以形成，以至于造成水泥凝结时间缩短、早期强度降低。
研究了不同养护温度（20℃、65℃及90℃）和不同养护湿度（干燥养护、密封养护及浸水养护）下原生型无水石膏在水泥中作用效果的变化规律，发现养护温度会影响原生型无水石膏在水泥中的最佳掺量，经历了早期高温养护的原生型无水石膏水泥在水化后期仍有较好的体积稳定性，但其生成延迟性钙钒石的风险要高于二水石膏水泥；养护湿度对原生型无水石膏水泥宏观性能的影响与二水石膏水泥类似，但原生型无水石膏在低成型水灰比且干燥养护条件下反应更慢，水化28d时依然有少量无水石膏存在，增加了产生延迟性钙矾石的风险。
In recent years, the content of protogenetic sulfate in cement clinker and admixturebecomes higher and higher. However, in order to avoid negative effects resulted bysulfate, the SO3content in cement clinker and admixture is limited by almost allcountries, which makes the cement clinker with high sulfate and pozzolanic sludge withhigh sulfate difficult for the production of cement. In situations such as this, if thesulfate in cement clinker and admixture can substitute for the gypsum added as cementretarder, and there is no need to limit the SO3content in cement clinker and admixture,it just needs to limit the total SO3content of cement. Sulfate minerals in cement clinkerare mainly alkaline metal sulfate, double salt, sulphoaluminate and anhydrite. Sulfateminerals in admixtures are mainly anhydrite. In so many types of protogenetic sulfate,the anhydrite existed in cement clinker and admixture has the most similar performancewith dihydrate gypsum. Therefore, whether protogenetic anhydrite can play the role ofdihydrate gypsum in cement is a precondition for the reasonable use of protogeneticanhydrite and other types of protogenetic sulfate in cement production.
Firstly, the types and content of protogenetic anhydrite in cement clinker andadmixtures were analyzed. The results show that protogenetic anhydrite is mainlyexisted in coal combustion waste. The dissolution rate of protogenetic anhydrite islower than that of dihydrate gypsum, but the dissolubility of the former is higher thanthat of the latter. By comparing dissolution property of calcined gypsum produced indifferent technology, it found that calcined gypsums by using natural dihydrate gypsumcalcined at850℃temperature for2hours and at1200℃for0.5hours can be used tosimulate protogenetic anhydrite.
Influence of protogenetic anhydrite on physical-mechanical properties of Portlandcement by mixing cement clinker with various contents of protogenetic anhydrite wasresearched. The results show that protogenetic anhydrite does not much affect waterrequirement of standard consistency of Portland cement, but significantly affect thesetting time of Portland cement. The effect of protogenetic anhydrite on settingretarding of cement is stronger than natural anhydrite, but slightly weaker thandihydrate gypsum. Protogenetic anhydrite can remarkably improve the early strength ofcement, and improvement effect is a median between natural anhydrite dihydrategypsum. Protogenetic anhydrite can reduce drying-shrinkage of cement, and the effect of protogenetic anhydrite on compensating shrinkage of cement is almost the same asthat of dihydrate gypsum, but is better than that of natural anhydrite. The research abouthydration process shows that protogenetic anhydrite releases sulphate ion which canform ettringite in the cement solution, and ettringite inhibits the quick hydration of C_3A,so that retards cement hydration. The formation of ettringite improves the early strengthof the cement and reduces dry-shrinkage of cement. Compared with dihydrate gypsum,the dissolution rate of protogenetic anhydrite is too slow to result in the lower sulphateion concentration in the early time of hydration. In addition, the formation of ettringiteis less and later. So the effect of protogenetic anhydrite on inhibition hydration of C_3Ais weaker than dihydrate gypsum.
The cements with different C_3A and alkali content were obtained by adding C_3Aand solid natrium hydroxide in cement. On that basis, the influence of cementcomposition on the role of protogenetic anhydrite in Portland cement was studied. Theresults show that the effect of protogenetic anhydrite on cement hydration andhardening is closely related to cement composition. When the C_3A and alkali content incement is higher, the setting retarding effect of protogenetic anhydrite is reduced. Andfor high C_3A (about12%) or high alkali (about1.7%) cement, it can't effectivelyprolong the setting time of cement by adding a certain amount of protogenetic anhydrite.Compared with dihydrate gypsum, protogenetic anhydrite in cement with high C_3A andhigh alkali can't effectively improve the early strength of cement. In cement includinghigh C_3A and high alkali content, the dissolution rate of protogenetic anhydrite is lowerthan the consumption rate of sulphate ion, so that sulphate ion concentration is lowerand the formation of AFt becomes difficulty, that cause the setting time of cementshortened, and the early strength reduced.
The changing rule of the role of protogenetic anhydrite in Portland cement underdifferent curing temperature (including20℃,65℃and90℃) and curing humidity(including dry-curing, seal-curing and water-curing). The results show that curingtemperature will affect the optimum dosage of protogenetic anhydrite in cement.Cement produced by protogenetic anhydrite under high temperature curing in early-agestill has better volume stability in the long age, but the risk of formation of delayedettringite is higher than that of cement produced by dihydrate gypsum. The influence ofcuring humidity on physical-mechanical properties of protogenetic anhydrite issimilarly to that of dihydrate gypsum cement. But the dissolution and hydration ofprotogenetic anhydrite under dry-curing condition become much slower, so that there is still some unreacted anhydrite in cement paste at28-days age, which increases the riskof formation of delayed ettringite.
引文
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ZI玉硬..ia nn aM华根t偿会碱a,f.宝,VC,r,石Ko邵童l硫e..TJi nule o cmuoI.收张对ekr膏Rr低,t水洪大n酸二kmn石engSa J淑缩钙Ph水泥江懋c水钙r,水et oh.e D膏e混caE珍矾D化cf灰石,.o在x硫:afh h.rf pBae等不Iffp凝,石物比的盐酸n活en awJscm,gfn等.同u土Plt理结Hs性Ci对孔lf酸i钙.eus sa含i石e.ooo a中-晶S及化tn硅结t和n和关,nTfrfa超yce膏rhs延及ec酸构s耐氯氢t[ehee学于t Mo细d s影eo o迟溶un盐ema久与n化氧]f-ct硬矿el.应.W响eri钙t解水c力t钠t性A化Tehmh渣o石r用t eh蒸Ceoe钒p性研dr泥学水钙膏e so[te[水.Cyre石m养trM能vD水r性h溶l究a在作iepa]ua泥e.ee硅tc]y生uo的.[we水s化能lDo液d高Pst or杨成影o的uTir酸egf程or的g]中浓泥e ncea水e.flc盐i f an得对响e度aaf关c的tt武oNleda缓化nnrlcr水d li其u山[d的系溶nJ汉ia凝didruiO研eb]dg性nP泥cmml,.i影[e解igH译a理剂zhtoee南能euJ究t]bn制o-sa响度ic.工d.Ktuvvha机京n l f[ir品lei的a中bs混JOo大ot[[f h]hlJJandh理e.Hr工ie]强]影国d凝toiu.nef. co学m建o-的ffg a业cH度o河土f油o建响rlo i,c u筑nm,探2dc2op大mTOr的与e北田筑[intra0tJht材hh com讨tb0y]学io体机工.uo9理水e化[ser p mie o料nesn系n:J水学1tt理n工r业泥t学aett.]iert s学9o i.etE中p泥报-mr研e出n大制a,hTnn sf2中e报1igf tea的s基0,x究学oe版e品t.9lttstfihc国2c,e9ftuoo t溶复[r学,1s0h4rb社na ur J o建0ne19a,d]nla cf解合[e7o报99.n1ldt,M n1u筑,clS98d1o材s武u2ge度dhr(39ye,o(]4eryr材98iy料自.s,1dv汉n()n和dmo75I料i((:g:il然43t)n crfclp3工a1科eei)C)稳h:o4p1科to::ts科ime3n5e4h学s62业o-定Si7-reLio-0ner-学学u3i-1ot9-i1n大dm性e与4Us4H1.ot-svd研17,:f版5n2学L[go技.Po.0Pha.iJ)el究tono5ne]you术,学ldd.r n.dr[c2ttdtJi院lhr0化oa报l]t,aSoae e0.nnt院1nn mtam7工eC[9td,,d dJ,1iep1]刊9c es2进c9m.ae9s[9ete9r9trP,,m e9yma(展J6vr11nt]74e,aou9oe0..) t,n1rcn rf:8:Eiae2e45t8t o1cn [n0ea(eu1uJ.9des4d]0mn-7s ris).96Cgodn-:te11C,3eyce ogn2(.,3miren1986,11(11-12):1183–1200.st2a0-003,33(3):387-395.msact1)poe,.:inr eo6fW e4r nn.itatt1neh,at3i sueaR2th.i rn0ae7edi0lnsst he3g[sCJa.t te]Ioor.nacnn mCthce D,rer-e1ncmt C9aueetr9,niR i5o1nte,n9g as2a6necl50dao(Cr: n6Cco6d)h5o:ni1,9tng i21-ocr639ern9e7s9[ts4-J5e1],. o.2R2nC4e55ets(h.4meea)e:r Cnc9thh0,ae31nm-d99i90sC7t4ro,.y n3co1rf(e5Ct)e:e R6m9ee5sne-t7a, r0Pc2ha.,r i1s,99169,8206,(31:0Ⅵ):
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ZI玉硬..ia nn aM华根t偿会碱a,f.宝,VC,r,石Ko邵童l硫e..TJi nule o cmuoI.收张对ekr膏Rr低,t水洪大n酸二kmn石engSa J淑缩钙Ph水泥江懋c水钙r,水et oh.e D膏e混caE珍矾D化cf灰石,.o在x硫:afh h.rf pBae等不Iffp凝,石物比的盐酸n活en awJscm,gfn等.同u土Plt理结Hs性Ci对孔lf酸i钙.eus sa含i石e.ooo a中-晶S及化tn硅结t和n和关,nTfrfa超yce膏rhs延及ec酸构s耐氯氢t[ehee学于t Mo细d s影eo o迟溶un盐ema久与n化氧]f-ct硬矿el.应.W响eri钙t解水c力t钠t性A化Tehmh渣o石r用t eh蒸Ceoe钒p性研dr泥学水钙膏e so[te[水.Cyre石m养trM能vD水r性h溶l究a在作iepa]ua泥e.ee硅tc]y生uo的.[we水s化能lDo液d高Pst or杨成影o的uTir酸egf程or的g]中浓泥e ncea水e.flc盐i f an得对响e度aaf关c的tt武oNleda缓化nnrlcr水d li其u山[d的系溶nJ汉ia凝didruiO研eb]dg性nP泥cmml,.i影[e解igH译a理剂zhtoee南能euJ究t]bn制o-sa响度ic.工d.Ktuvvha机京n l f[ir品lei的a中bs混JOo大ot[[f h]hlJJandh理e.Hr工ie]强]影国d凝toiu.nef. co学m建o-的ffg a业cH度o河土f油o建响rlo i,c u筑nm,探2dc2op大mTOr的与e北田筑[intra0tJht材hh com讨tb0y]学io体机工.uo9理水e化[ser p mie o料nesn系n:J水学1tt理n工r业泥t学aett.]iert s学9o i.etE中p泥报-mr研e出n大制a,hTnn sf2中e报1igf tea的s基0,x究学oe版e品t.9lttstfihc国2c,e9ftuoo t溶复[r学,1s0h4rb社na ur J o建0ne19a,d]nla cf解合[e7o报99.n1ldt,M n1u筑,clS98d1o材s武u2ge度dhr(39ye,o(]4eryr材98iy料自.s,1dv汉n()n和dmo75I料i((:g:il然43t)n crfclp3工a1科eei)C)稳h:o4p1科to::ts科ime3n5e4h学s62业o-定Si7-reLio-0ner-学学u3i-1ot9-i1n大dm性e与4Us4H1.ot-svd研17,:f版5n2学L[go技.Po.0Pha.iJ)el究tono5ne]you术,学ldd.r n.dr[c2ttdtJi院lhr0化oa报l]t,aSoae e0.nnt院1nn mtam7工eC[9td,,d dJ,1iep1]刊9c es2进c9m.ae9s[9ete9r9trP,,m e9yma(展J6vr11nt]74e,aou9oe0..) t,n1rcn rf:8:Eiae2e45t8t o1cn [n0ea(eu1uJ.9des4d]0mn-7s ris).96Cgodn-:te11C,3eyce ogn2(.,3miren1986,11(11-12):1183–1200.st2a0-003,33(3):387-395.msact1)poe,.:inr eo6fW e4r nn.itatt1neh,at3i sueaR2th.i rn0ae7edi0lnsst he3g[sCJa.t te]Ioor.nacnn mCthce D,rer-e1ncmt C9aueetr9,niR i5o1nte,n9g as2a6necl50dao(Cr: n6Cco6d)h5o:ni1,9tng i21-ocr639ern9e7s9[ts4-J5e1],. o.2R2nC4e55ets(h.4meea)e:r Cnc9thh0,ae31nm-d99i90sC7t4ro,.y n3co1rf(e5Ct)e:e R6m9ee5sne-t7a, r0Pc2ha.,r i1s,99169,8206,(31:0Ⅵ):